A method for ultraviolet sterilization, negative pressure dust removal and layering of sports nutrition powder in vitro packaging
Patent Information
- Application Number
- CN202611174354.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2026-08-04
- Publication Date
- 2026-09-29
AI Technical Summary
[0003]植物原料中的酚酸类成分和黄酮类成分在溶出速度、适宜溶剂组成及树脂吸附能力方面存在差异,以固定时间或单一标志成分控制提取时,可能出现一种成分已接近提取完全,而另一种成分仍具有回收价值的情况;延长提取又会使糖类、蛋白质及其他非目标固形物继续溶出,导致后续树脂上样负荷增加,不同目标成分在吸附分离柱中的穿透次序及洗脱区间也可能不同,固定采用单柱或双柱串联上样时,先发生穿透的成分容易随流出液损失;将串联柱整体洗脱或者按照液体体积直接合并流份时,又难以消除不同馏分固形物含量差异造成的成分比例偏移,所得提取物粉体的批次组成因而不易保持稳定
1、本发明通过在各循环支路汇流前分别检测酚酸类目标标志成分、黄酮类目标标志成分、可溶性固形物及循环流量,扣除与当前提取级相对应的溶剂背景,并结合两类目标标志成分的质量流率、增量回收状态以及相对于共提固形物的提取选择性确定目标富集流份和提取终点,达到同时兼顾两类目标标志成分回收程度和非目标固形物共提负荷的效果,减少固定时间提取造成的过度提取,也可避免仅依据一种目标标志成分确定终点时另一种目标,标志成分尚未充分溶出的情况。
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Abstract
Description
Technical Field
[0001] This invention belongs to the field of natural product active ingredient extraction and powder processing technology, specifically a method for ultraviolet sterilization, negative pressure dust removal, and layered feeding and mixing of sports nutrition powder in its outer packaging. Background Technology
[0002] Extracts of active ingredients from natural products are often used as functional raw materials for sports nutrition powders. Current production typically involves drying, pulverizing, and extracting plant materials such as mulberry leaves, hawthorn leaves, and honeysuckle with an ethanol-water solution. The extract powder is then obtained through adsorption with macroporous adsorption resin, gradient elution with ethanol, concentration, and drying. The extraction process and endpoint are often determined according to a preset time or based on changes in the concentration of a single marker component and the solid content of the extract. The resin separation process usually employs a fixed sample loading amount, a fixed column connection method, and a preset elution range.
[0003] Phenolic acids and flavonoids in plant raw materials differ in terms of dissolution rate, suitable solvent composition, and resin adsorption capacity. When extraction is controlled by a fixed time or a single marker component, one component may be nearly completely extracted while another still has recovery value. Extending the extraction time will cause sugars, proteins, and other non-target solids to continue to dissolve, leading to an increase in the loading load on the subsequent resin. The breakthrough order and elution range of different target components in the adsorption separation column may also be different. When using a single column or dual columns in series for loading, the component that breaks through first is easily lost with the effluent. When eluting the entire column in series or directly combining fractions according to liquid volume, it is difficult to eliminate the component ratio shift caused by the difference in solid content of different fractions, and the batch composition of the obtained extract powder is therefore not easy to maintain stability.
[0004] After the active ingredient extract powder is packaged, temporarily stored, or transported across regions, it still needs to enter the clean feeding and mixing process. In the current production, raw material batches, extraction processes, resin column usage records, powder moisture content, marker component content, packaging cleanliness status, and actual feeding objects are usually managed in segments. The correspondence between the front-end test results and the actual feeding and packaging at the back end may be interrupted. If the feeding amount is determined according to the total powder mass or the content of a single marker component, there may be a situation where one marker component is within the allowable range, while another marker component is insufficient or excessive. Residual dust on the packaging surface may also enter the clean area when the package is unpacked and fed. The above problems will be reflected simultaneously as loss of target component recovery, increased load of non-target solids, fluctuations in the composition of extracts between batches, and deviations in the amount of active ingredient added in the finished product. Summary of the Invention
[0005] The dissolution rates, suitable extraction conditions, and adsorption and penetration behaviors of phenolic acid and flavonoid components in plant natural product raw materials vary. If extraction is completed at a fixed time or the extraction endpoint is determined only based on the concentration change of one target marker component, there may be a situation where one target marker component is almost completely extracted, while another target marker component still has recovery value. Continuing to extend the extraction time will increase the co-extraction of sugars, proteins and other soluble substances, and increase the processing load of subsequent adsorption and separation.
[0006] The breakthrough order and elution range of phenolic acid target markers and flavonoid target markers in the adsorption separation column are not completely consistent. If the loading endpoint is determined based on only one of the target markers, the target marker that breaks through first is easily lost with the eluent. If the adsorption separation columns in series are eluted as a whole, the target markers received by different adsorption separation columns will be concentrated in different elution ranges, making it difficult to adjust the content ratio of the two types of target markers in the final effective ingredient extract powder according to the actual composition of each eluent.
[0007] The active ingredient extract powder needs to go through multiple processing steps from extraction and separation, powder packaging, packaging surface purification to the clean feeding position. If the extraction and separation record, powder moisture content, and target marker component content formed at the front end do not correspond to the inner sealed packaging of the actual feeding, the feeding amount determined according to the front end test results may be incorrectly used for other batches of powder, thus affecting the actual amount of active ingredients added to the sports nutrition powder.
[0008] To address the aforementioned problems, this invention provides a method for ultraviolet sterilization, negative pressure dust removal, and layered feeding and mixing of sports nutrition powder in its outer packaging. The sports nutrition powder comprises an effective ingredient extract powder and a base powder made from plant natural product raw materials. This method identifies target enriched fractions with recovery value through graded cyclic extraction. The target marker components that first penetrate are sequentially introduced through a first adsorption separation column and a second adsorption separation column. After separate elution, the merging ratio is re-determined based on the actual component content of each eluted fraction. After packaging and purification, the amount of active ingredient extract powder is determined based on the actual content of phenolic acid target marker components and flavonoid target marker components, along with the final layer correction amount.
[0009] Plant natural product raw materials are placed in an extraction unit for at least two stages of cyclic extraction. When multiple extraction units are set up, each extraction unit has a circulation branch. Each circulation branch remains independent before merging into a common collection pipeline. The concentrations of phenolic acid target marker components, flavonoid target marker components, soluble solids concentration, extraction temperature, and circulation flow rate in the extract are detected upstream of the confluence point, so that the detection results can correspond to the corresponding extraction unit, plant natural product raw material batch, and extraction stage.
[0010] Before each extraction stage begins, a blank solvent with the same composition as the extraction solvent used in the current extraction stage is passed through the cleaned extraction unit and circulation branch. Detection values are continuously obtained under the same extraction liquid temperature, circulation flow rate, and sampling cycle as the actual extraction. The solvent background value of each target marker component and the solvent background value of soluble solids are determined based on the average value of the continuous detection values. The allowable range of the corresponding solvent background is determined based on the positive fluctuation of the continuous detection values relative to the corresponding average value.
[0011] In the actual extraction process, the solvent background value of the target marker component is subtracted from the detection concentration of the target marker component to obtain the effective detection concentration of the target marker component; the solvent background value of the soluble solids is subtracted from the detection concentration of the soluble solids to obtain the effective detection concentration of the soluble solids. By using the solvent background value corresponding to the actual extraction conditions, the influence of different ethanol volume fractions, extraction liquid temperature and circulation branch residues on the detection results can be reduced.
[0012] Based on the effective detection concentration and circulation flow rate of each target marker component, the mass flow rate of phenolic acid target marker components and flavonoid target marker components through the circulation branch per unit time was determined; based on the effective detection concentration and circulation flow rate of soluble solids, the mass flow rate of co-extracted solids through the circulation branch per unit time was determined.
[0013] The extraction selectivity of the current extract is characterized by the ratio of the sum of the mass flow rates of phenolic acid target marker components and flavonoid target marker components to the mass flow rate of the co-extracted solids. This extraction selectivity is used to reflect the enrichment degree of the target marker components in the current extract relative to other solids that are dissolved at the same time, avoiding the assumption that the corresponding fraction is suitable for collection simply because the concentration of the target marker components is high.
[0014] The extraction mass of phenolic acid target marker components and flavonoid target marker components in each detection period is accumulated, and the incremental recovery status of the corresponding target marker components is determined based on the increase in the cumulative extraction mass between adjacent detection periods. The incremental recovery status is used to reflect the increase in the recovery of target marker components that can be achieved by continuing to maintain the current extraction stage.
[0015] When the extraction selectivity is not lower than the fraction collection threshold and the mass flow rate of at least one target marker component is not lower than the corresponding collection lower limit, the corresponding extract is diverted to the target enrichment fraction pipeline. Extracts that do not meet the target enrichment fraction collection conditions are not included in the target enrichment fraction and are returned to the extraction unit for continued circulation according to the current process status of the extraction stage, or collected separately as a fraction to be recovered.
[0016] When the incremental recovery of both phenolic acid target marker components and flavonoid target marker components is not higher than their respective extraction endpoint thresholds, the extraction selectivity is not higher than the endpoint selectivity threshold, and the above conditions continue to last for the endpoint determination time, the current extraction stage ends. This ensures that the extraction endpoint is simultaneously constrained by the remaining recovery amount of the target marker components and the co-extracted solids load, reducing the situation where the increase in target marker components from continued extraction is limited while the co-extracted substances continue to increase.
[0017] After the current batch of plant natural product raw material extraction is completed, the corresponding extraction unit and circulation branch are rinsed with cleaning solvent. When the detection values of phenolic acid target marker components, flavonoid target marker components, and soluble solids are all restored to the allowable range of their respective solvent backgrounds and continue to reach the signal reset time, the extraction of the next batch of plant natural product raw material is then started. This is to reduce the impact of the residual extract from the previous batch on the detection results of the next batch and the determination of the extraction endpoint.
[0018] In one embodiment, the plant natural product raw material is selected from mulberry leaves, hawthorn leaves, and honeysuckle. When the plant natural product raw material is mulberry leaves, the target marker component for phenolic acids is chlorogenic acid, and the target marker component for flavonoids is rutin or isoquercitrin. When the plant natural product raw material is hawthorn leaves, the target marker component for phenolic acids is chlorogenic acid, and the target marker component for flavonoids is hyperoside. When the plant natural product raw material is honeysuckle, the target marker component for phenolic acids is chlorogenic acid, and the target marker component for flavonoids is luteolin.
[0019] The plant natural product raw materials are sequentially subjected to impurity removal, drying, pulverization, and sieving. The drying temperature is not higher than 60 degrees Celsius. The particle size of the pulverized plant natural product raw materials is 20-60 mesh, and the moisture content is not higher than 12%. The first-stage cyclic extraction uses an ethanol aqueous solution with an ethanol volume fraction of 20%-45%, and the second-stage cyclic extraction uses an ethanol aqueous solution with an ethanol volume fraction of 45%-70%. The ethanol volume fraction used in the second-stage cyclic extraction is higher than that used in the first-stage cyclic extraction.
[0020] Each circulation branch is equipped with an online spectral detection component, a refractive index detection component, a temperature detection component, and a circulation flow detection component. The online spectral detection component uses a calibration model established according to the type of plant natural product raw material and the extraction grade to determine the detection concentration of each target marker component in the extract.
[0021] The calibration model is established using target marker component standards, extract samples of corresponding plant natural product raw materials, and high-performance liquid chromatography detection results. Validation samples not involved in the establishment of the calibration model are used to determine the applicable concentration range and prediction error of the calibration model. Only when the prediction error of the calibration model is within the allowable range under the corresponding plant natural product raw materials and extraction stage is its output result used for fraction allocation and extraction endpoint determination.
[0022] The refractive index obtained by the refractive index detection component is compensated based on the current ethanol volume fraction and temperature of the extract, and then converted into soluble solids concentration. When the target marker component detection concentration or soluble solids concentration is lower than the corresponding lower limit of quantitation, the corresponding detection results are not used to determine the mass flow rate and extraction selectivity. When the extract temperature or circulation flow rate exceeds the corresponding stable range, the use of data from the corresponding detection period to determine the target enriched fraction and extraction endpoint is suspended.
[0023] The target enriched fractions formed from the same batch of plant natural product raw materials are combined, and ethanol is recovered by adding water or reducing pressure to ensure that the volume fraction of ethanol in the combined target enriched sulfur fraction is not higher than 15%. The target enriched fractions are then sent to the first adsorption separation column.
[0024] The first and second adsorption separation columns are respectively filled with non-polar or weakly polar macroporous adsorption resins selected by the adsorption test of the target marker components, and the valve group switches between the state of individual sample loading on the first adsorption separation column and the state of sample loading in series between the first adsorption separation column and the second adsorption separation column.
[0025] During the individual sample loading of the first adsorption separation column, the concentrations of phenolic acid target marker components and flavonoid target marker components before and after the first adsorption separation column are detected respectively. The breakthrough state is determined according to the ratio of the post-column concentration of each target marker component to the corresponding pre-column concentration. The component that first reaches the first breakthrough threshold among the phenolic acid target marker components and flavonoid target marker components is determined as the first breakthrough target marker component.
[0026] When the target marker component penetrates to the first penetration threshold, the second adsorption separation column is connected downstream of the first adsorption separation column through the valve assembly, so that the effluent from the first adsorption separation column enters the second adsorption separation column. The second adsorption separation column continues to adsorb the target marker component that has already penetrated from the first adsorption separation column, which can reduce the degree of loss of the target marker component with the effluent from the first adsorption separation column.
[0027] After the second adsorption separation column is connected, the concentrations of phenolic acid target marker components and flavonoid target marker components in the effluent of the second adsorption separation column are detected. When any target marker component in the effluent of the second adsorption separation column reaches the second breakthrough threshold, or when the target enrichment fraction of the current batch of plant natural product raw materials is loaded, the loading is stopped. The second breakthrough threshold is lower than the first breakthrough threshold, so that the second adsorption separation column stops receiving the target enrichment fraction before the target marker component shows obvious breakthrough.
[0028] After the sample loading was completed, the series connection between the first adsorption separation column and the second adsorption separation column was broken. The first adsorption separation column and the second adsorption separation column were washed with water, eluted with low-concentration ethanol aqueous solution and high-concentration ethanol aqueous solution respectively. The volume fraction of ethanol in the high-concentration ethanol aqueous solution was higher than that in the low-concentration ethanol aqueous solution.
[0029] The content of phenolic acid target marker components, flavonoid target marker components, and dried solids in each elution interval of the first and second adsorption separation columns is detected. The eluents from the first and second adsorption separation columns with a higher mass fraction of phenolic acid target marker components relative to dried solids are combined into the first elution fraction; the eluents with a higher mass fraction of flavonoid target marker components relative to dried solids are combined into the second elution fraction. The division of the first and second elution fractions is based on the actual composition of the eluents and does not correspond to the first and second adsorption separation columns respectively.
[0030] The mass fractions of phenolic acid target marker components and flavonoid target marker components, based on the mass of dry solids contained in the first eluent and the second eluent sulfur fraction, are determined respectively. Multiple candidate merging ratios are formed according to a preset ratio step size between the mass of dry solids contained in the first eluent and the mass of dry solids contained in the second eluent.
[0031] Based on the mass of dried solids and the mass of each target marker component provided by the first and second elution fractions under each candidate merging ratio, the mass fractions of phenolic acid target marker components and flavonoid target marker components in the merged dried solids are determined, and candidate merging ratios that ensure both mass fractions are within the corresponding batch control range are selected.
[0032] The batch control range is determined based on the product quality requirements of the active ingredient extract powder or the verified production process control requirements. When there are multiple candidate merging ratios that meet the batch control range, the deviation of each target marker component from the median of its respective batch control range is normalized according to the width of the corresponding batch control range, and the candidate merging ratio with the smaller sum of normalized deviations is selected.
[0033] If there is no candidate merging ratio that can simultaneously satisfy the corresponding batch control range for phenolic acid target marker components and flavonoid target marker components, the corresponding elution fraction is not directly used to prepare active ingredient extract powder. Instead, the ethanol volume fraction of at least one elution fraction is adjusted to a range suitable for adsorption by macroporous adsorption resin and then sent to a re-adsorption separation pipeline connected to the sample pipeline of the adsorption separation column.
[0034] The first and second elution fractions were combined according to the determined merging ratio, and then concentrated and dried under reduced pressure to obtain an effective ingredient extract powder in which both the phenolic acid target marker component and the flavonoid target marker component were within the corresponding batch control range.
[0035] The moisture content of the active ingredient extract powder was tested, and the dry mass fraction of phenolic acid target marker components and flavonoid target marker components was tested based on the dry powder mass. After passing the test, the active ingredient extract powder was packed into an inner sealed package. The inner sealed package is the direct outer packaging that is in direct contact with the active ingredient extract powder. An outer paper package for transportation and storage protection was then placed over the inner sealed package.
[0036] Establish an extraction and separation record corresponding to the inner sealed packaging. The extraction and separation record includes the name of the plant natural product raw material, the batch of the plant natural product raw material, the extraction grade, the target enrichment fraction range, the first adsorption separation column number, the second adsorption separation column number, the elution fraction merging ratio, the dry mass fraction of the phenolic acid target marker component, the dry mass fraction of the flavonoid target marker component, and the powder moisture content. The material information of the inner sealed packaging includes the name of the active ingredient extract powder, the batch of the active ingredient extract powder, and the net content of the packaging.
[0037] Before the inner sealed packaging enters the sterilization and dust removal tunnel, the outer surface of the outer paper packaging is cleaned and disinfected. After there are no more disinfectant drips on the surface of the outer paper packaging, the outer paper packaging is removed outside the sterilization and dust removal tunnel, and the inner sealed packaging is checked for any open seals, packaging damage, or powder leakage.
[0038] Place the inner sealed packaging that has passed the integrity check at the conveyor location marked with a location identifier, and link the material information and corresponding extraction and separation records of the inner sealed packaging with the location identifier. This ensures that the actual target component content of the corresponding batch can always be retrieved during the conveying process of the active ingredient extract powder from the packaging purification to the clean feeding position.
[0039] The sterilization and dust removal tunnel is equipped with multiple dust removal sections along the inner sealed packaging conveying direction. The exhaust ports of each dust removal section are connected to the common exhaust pipe through exhaust branch lines. The particulate matter detection component samples each exhaust branch line before it merges into the common exhaust pipe, so that the particulate matter detection results can be mapped to specific dust removal sections and specific conveying locations.
[0040] Control the conveying interval of adjacent inner sealed packaging so that each dust removal section corresponds to one inner sealed packaging during the dust removal judgment period. When performing background detection, the dust removal section is in an unloaded state, and multiple background particulate matter detection values are continuously obtained according to the actual dust removal air volume, exhaust volume and sampling cycle.
[0041] The average value of multiple background particulate matter detection values is determined as the background particulate matter detection value. The maximum positive deviation of each background particulate matter detection value from the average value is determined as the background fluctuation amount. The sum of the background particulate matter detection value and the background fluctuation amount is determined as the upper limit of dust removal judgment.
[0042] After the inner sealed packaging enters the corresponding dust removal section, clean airflow is delivered to the outer surface of the inner sealed packaging through the air outlet, and the airflow carrying dust on the packaging surface is extracted through the exhaust branch. When the detected value of the processed particulate matter is not higher than the upper limit of the dust removal judgment and continues to reach the dust removal judgment time, the corresponding inner sealed packaging is determined to have completed dust removal.
[0043] After the previous inner sealed package leaves the dust removal section, the corresponding exhaust branch continues to operate. When the particle detection value is not higher than the upper limit of dust removal judgment and continues to reach the signal reset time, the next inner sealed package is allowed to enter the corresponding dust removal section, so as to reduce the impact of the residual dust-laden airflow generated by the previous inner sealed package on the dust removal judgment of the next inner sealed package.
[0044] The ultraviolet irradiation assembly includes a top ultraviolet irradiation unit located above the conveying path and side ultraviolet irradiation units located on both sides of the conveying path. Starting from the time when the inner sealed packaging completes dust removal, the ultraviolet irradiation amount obtained after the inner sealed packaging completes dust removal is accumulated based on the calibrated irradiation intensity of each ultraviolet irradiation unit and the time it takes for the inner sealed packaging to pass through the corresponding irradiation range.
[0045] Packaging samples made of the same material as the inner sealing packaging were subjected to ultraviolet irradiation and microbial testing on the packaging surface. The minimum ultraviolet irradiation threshold corresponding to the microbial test results on the packaging sample surface meeting the release requirements of the packaging surface in the production site was determined as the ultraviolet irradiation threshold for the corresponding packaging material.
[0046] The material information of the inner sealed packaging, the extraction and separation record, the dust removal completion result, and the ultraviolet irradiance obtained after dust removal are linked with the corresponding load position marker. After the inner sealed packaging reaches the clean feeding position, the material information and the corresponding load position marker of the inner sealed packaging are read.
[0047] When the read material information is consistent with the material information associated with the location identifier, the corresponding dust removal completion result indicates that dust removal has been completed. When the ultraviolet irradiance obtained after dust removal reaches the ultraviolet irradiance threshold, the locking state of the corresponding feeding execution component is released. If any condition is not met, the corresponding feeding execution component remains locked, and the corresponding inner sealed packaging is sent to the isolation position.
[0048] When determining the target feed amount of active ingredient extract powder, the dry mass fractions of phenolic acid target marker components and flavonoid target marker components are converted into the mass fractions of active ingredient extract powder under actual moisture content, based on the powder moisture content.
[0049] Based on the lower and upper limits of the allowable input of phenolic acid target marker components specified in the formula, as well as the mass fraction of phenolic acid target marker components in the actual water content state of the active ingredient extract powder, the first powder input mass range that meets the input requirements of phenolic acid target marker components is determined.
[0050] Based on the lower and upper limits of the allowable input of the flavonoid target marker components specified in the formula, as well as the mass fraction of the flavonoid target marker components in the actual water content state of the active ingredient extract powder, a second powder input mass range that meets the input requirements of the flavonoid target marker components is determined.
[0051] The overlapping portion of the first and second powder feedable mass ranges is defined as the allowable feed mass range. If there is no overlapping portion, it indicates that adjusting the feed mass of the current batch of active ingredient extract powder alone cannot simultaneously meet the formulation requirements for phenolic acid target marker components and flavonoid target marker components. In this case, the corresponding feeding execution component is locked.
[0052] When there is an allowable feed mass range, the corresponding reference feed mass is determined according to the nominal feed amount of the phenolic acid target marker component and the flavonoid target marker component, respectively. The mass with the smaller overall deviation from the two reference feed masses is selected from the allowable feed mass range as the target feed amount.
[0053] Based on the target feeding amount of the active ingredient extract powder and the target feeding amount of the base powder, the active ingredient extract powder is distributed to at least two feeding layers. The base powder is preferentially fed between two adjacent feedings of the active ingredient extract powder, so that the active ingredient extract powder is distributed in the base powder in an intermittent manner.
[0054] After the current feeding layer has finished feeding, the shared feeding and conveying path continues to operate. When the residual material detection component set at the discharge end of the shared feeding and conveying path does not detect the passage of powder material during the continuous detection period, it is determined that the powder material of the current feeding layer has been discharged, and then the next feeding layer begins, thereby reducing the overlap of materials between adjacent feeding layers in the shared feeding and conveying path.
[0055] Before the last feeding layer begins, the cumulative actual amount of phenolic acid target markers and the cumulative actual amount of flavonoid target markers are determined based on the cumulative actual amount of active ingredient extract powder in the previous feeding layers, the powder moisture content, and the dry mass fraction of phenolic acid target markers and flavonoid target markers.
[0056] Based on the difference between the cumulative actual input of phenolic acid target marker components and the corresponding allowable input range, the quality range for supplementary input in the final layer corresponding to the phenolic acid target marker components is determined; based on the difference between the cumulative actual input of flavonoid target marker components and the corresponding allowable input range, the quality range for supplementary input in the final layer corresponding to the flavonoid target marker components is determined.
[0057] The overlapping portion of the two final layer replenishable mass intervals is defined as the final layer allowable corrective feeding mass interval. When a final layer allowable corrective feeding mass interval exists, the final layer corrective feeding amount is determined from this interval. When a final layer allowable corrective feeding mass interval does not exist, or when the cumulative actual input amount of any target marker component has exceeded the corresponding allowable input limit, the corresponding feeding execution component is locked, and the mixing device is stopped.
[0058] When the cumulative actual input of phenolic acid target marker components and flavonoid target marker components are both within their respective allowable input ranges, and the residual material detection component confirms that the powder material of the last feeding layer has been discharged, the mixing device is started to mix.
[0059] The beneficial effects of this invention are as follows: 1. This invention detects phenolic acid target marker components, flavonoid target marker components, soluble solids, and circulation flow rate before each circulation branch merges, subtracts the solvent background corresponding to the current extraction stage, and determines the target enriched fraction and extraction endpoint by combining the mass flow rate, incremental recovery status, and extraction selectivity of the two types of target marker components relative to the co-extracted solids. This achieves the effect of simultaneously taking into account the recovery degree of the two types of target marker components and the co-extraction load of non-target solids, reducing over-extraction caused by fixed-time extraction, and also avoiding the situation where the other target marker component has not been fully dissolved when the endpoint is determined based on only one target marker component.
[0060] 2. This invention controls the second adsorption separation column to be connected downstream of the first adsorption separation column by the component that first reaches the first penetration condition among two types of target marker components. After the sample loading is completed, the series connection between the two columns is broken, and the first and second adsorption separation columns are eluted separately. Then, the composition and merging ratio of the eluent are determined according to the actual content of dried solids and the two types of target markers in each basic eluted sulfur fraction. This achieves the effect of receiving the target marker component that first penetrates, reducing its loss with the column effluent, and adjusting the composition of the final extract. It avoids the component ratio shift caused by fixing the two columns in series and directly merging according to the volume of the eluent, which is beneficial to maintaining the compositional stability of the effective component extract powder obtained from different batches of raw materials.
[0061] 3. This invention continuously correlates the raw material batch, extraction stage, target enrichment fraction, adsorption separation column number, elution fraction merging ratio, powder moisture content, and dry content of the two types of target marker components with the inner sealed packaging and conveying position. It also uses the packaging negative pressure dust removal result and ultraviolet irradiation as feeding release conditions. During the feeding stage, the target feeding amount is determined based on the overlapping part of the powder feeding mass range corresponding to the two types of target marker components. At the same time, the final feeding amount is corrected by combining the cumulative actual feeding amount. This achieves the effect of continuous correspondence between the front-end extraction and separation results, the packaging purification status, and the actual feeding objects at the back end. This reduces the risk of batch information mismatch and packaging surface contamination entering the clean feeding area, and ensures that the actual feeding amount of the two types of target marker components is within the allowable range specified in the formula. Attached Figure Description
[0062] Figure 1 This is an overall flowchart of the method for ultraviolet sterilization, negative pressure dust removal, and layered feeding and mixing of sports nutrition powder in the external packaging of the present invention. Figure 2 This is a block diagram of the overall structure of the sports nutrition powder preparation, packaging, purification, and feeding system of the present invention. Figure 3 This is a schematic diagram of the connection structure of the extraction unit and the loop branch of the present invention; Figure 4 Flowchart for solvent background detection, effective detection concentration, and extraction status determination; Figure 5 Flowchart for determining the enrichment of target fractions and extraction endpoints; Figure 6 The invention includes a flowchart for the breakthrough detection of the first adsorption separation column and the control flow for the connection of the second adsorption separation column; Figure 7 To develop a flow chart for column elution and elution fraction merging; Figure 8 A flowchart for the purification, information association, and final layer correction of the inner sealed packaging was invented. Detailed Implementation
[0063] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.
[0064] like Figures 1 to 8 Therefore, this embodiment is applicable to production conditions where the preparation area of plant natural product active ingredient extract powder and the clean mixing area of sports nutrition powder are separated. After the active ingredient extract powder is extracted, adsorbed and separated, concentrated, dried and sealed in the extract preparation area, it needs to be temporarily stored in batches or transported across regions before entering the clean mixing area. In order to ensure that the content of the target marker component obtained at the front end can be accurately used for the subsequent feeding of the corresponding batch of powder, and at the same time reduce the risk of dust and microorganisms on the surface of the transport packaging entering the clean feeding position, this embodiment keeps the extraction and separation records, inner sealing packaging, packaging purification records and layered feeding records continuously linked.
[0065] The following uses mulberry leaves as the main verification raw material, chlorogenic acid as the target marker component of phenolic acids, and rutin as the target marker component of flavonoids to describe the complete process. Hawthorn leaves and honeysuckle use the same control logic, but corresponding online detection models, solvent background, extraction endpoint, adsorption separation and elution parameters are established separately, and the quantitative parameters of mulberry leaves are not directly applied.
[0066] In this embodiment, the dry weight content of the target marker component is expressed as the dry weight mass fraction of the target marker component, that is, the proportion of the mass of the target marker component to the mass of the effective component extract powder after removing water. Soluble solids are the non-volatile substances obtained after removing volatile solvents from the extract under specified conditions. The target enriched fraction is the extract that meets the mass flow rate and extraction selectivity conditions of the target marker component and is collected by splitting. Extraction selectivity is used to characterize the degree of enrichment of the two types of target marker components relative to the co-extracted solids per unit time. Incremental recovery status is used to characterize the increased mass of target marker components obtained by continuing extraction within adjacent detection time windows.
[0067] The first and second penetration conditions are both determined based on the ratio of the concentration of the target marker component after the adsorption separation column to the concentration of the target marker component before the column at the same time. The first penetration condition is used to trigger the access of the second adsorption separation column, and the second penetration condition is used to limit the loss of the target marker component at the outlet of the second adsorption separation column. The first and second elution fractions are divided according to the actual composition of the basic elution fractions, and are not limited to coming from the first and second adsorption separation columns respectively.
[0068] Example 1: Production System Composition and Material Correspondence This embodiment employs a raw material pretreatment device, one or more extraction units, an extraction solvent supply device, a circulation detection device, a target enriched fraction collection device, a recoverable fraction collection device, a first adsorption separation column, a second adsorption separation column, an eluent supply device, a basic eluent fraction collection device, a concentration device, a vacuum drying device, a powder detection device, a packaging device, a sterilization and dust removal tunnel, a material conveying mechanism, a feeding execution component, a feeding conveying mechanism, a residual material detection component, and a mixing device.
[0069] Each extraction unit can sequentially perform the first-stage cyclic extraction and the second-stage cyclic extraction. When multiple extraction units are set up, each extraction unit processes different batches of plant natural product raw materials in parallel. The circulation branches of each extraction unit remain independent of each other before entering the common collection pipeline. The circulation branches are sequentially equipped with a circulation pump, filter components, circulation flow detection components, temperature detection components, online spectral detection components, refractive index detection components, ethanol volume fraction detection components, and diversion valves along the flow direction of the extract.
[0070] The diversion valves connect to the reflux port of the extraction unit, the target enrichment fraction pipeline, and the recovery fraction pipeline, respectively. When the extract is diverted, the solvent replenishment pipeline adds an equal volume of extraction solvent compatible with the current extraction stage to the extraction unit, maintaining the liquid level within the extraction unit within the set range. The ethanol volume fraction detection component is used to confirm the actual ethanol volume fraction of the extract. If the actual ethanol volume fraction deviates from the set range of the current extraction stage, it is corrected by adding ethanol or purified water. The detection data during the correction period is not used for target enrichment fraction distribution or extraction endpoint determination.
[0071] The first adsorption separation column and the second adsorption separation column each have an inlet, an outlet, a pre-column detection position, a post-column detection position, and a switching valve group. The switching valve group enables the system to be in the following states: sample loading state of the first adsorption separation column alone, sample loading state of the first adsorption separation column and the second adsorption separation column in series, and elution state of the first adsorption separation column and the second adsorption separation column independently. The post-column detection position of the first adsorption separation column is located upstream of the switching valve group. The pipeline volume between the detection position and the switching valve group is controlled within a transition volume that can be completely transferred within one sampling cycle.
[0072] The control device generates a batch identifier for each batch of plant natural product raw materials and sequentially writes the extraction unit number, extraction stage, target enrichment fraction range, first adsorption separation column number, second adsorption separation column number, basic elution fraction number, elution fraction merging ratio, active ingredient extract powder batch, inner sealed packaging identifier, and conveying carrier identifier into the same extraction and separation record. As a result, subsequent feeding uses the actual test data of the powder in the current inner sealed packaging, rather than the historical average value of the same type of powder.
[0073] Example 2: Pretreatment of mulberry leaf raw materials and two-stage extraction conditions Mulberry leaves, whose variety and source have been confirmed, are selected as raw materials for plant natural products. When accepting raw materials, the supply batch, harvest time and initial moisture content are recorded. Samples are taken from the top, middle and bottom of the batch, and after mixing, the initial contents of chlorogenic acid and rutin are tested. Different supply batches are identified separately, and raw materials from different batches are not mixed before extraction.
[0074] Mulberry leaves are first removed manually and using screening equipment to remove sand, gravel, dead branches, and non-target plant tissues. They are then dried at a temperature not exceeding 60 degrees Celsius. During the drying process, samples are taken at fixed time intervals to test the moisture content until it does not exceed 12%. The dried mulberry leaves are then pulverized and passed through a 20-mesh sieve, with some particles retained on a 60-mesh sieve. Coarse particles that do not pass through the 20-mesh sieve are re-pulverized; fine powder that passes through the 60-mesh sieve is collected separately and not directly entered into the circulating extraction circuit, thus reducing the amount of fine powder entering the circulating branch and adhering to the detection flow cell.
[0075] In this embodiment, 1000 grams of mulberry leaf raw material, calculated based on dry weight, is added per batch. The first-stage cyclic extraction uses a 35% (v / v) ethanol-water solution, establishing an actual liquid-to-solid ratio of 12 ml / g, with an extraction temperature of 55°C and a circulation flow rate of 6 L / min. The second-stage cyclic extraction uses a 60% (v / v) ethanol-water solution, establishing an actual liquid-to-solid ratio of 10 ml / g, with an extraction temperature of 55°C and a circulation flow rate of 5 L / min. After the first-stage cyclic extraction, the extraction unit is allowed to stand for 10 minutes to drain, and the drained liquid volume is recorded. Based on the estimated volume of residual liquid in the raw material support basket and the ethanol volume fraction in the mulberry leaf raw material, the ethanol volume fraction and addition amount of the second-stage extraction solvent are adjusted to ensure that the actual ethanol volume fraction after the second-stage cycle is between 58% and 62%. If the ethanol volume fraction does not fall within this range, the second-stage target enrichment fraction determination is not initiated.
[0076] Example 3: Online Spectral Calibration Model and Reference Detection The online spectral detection component adopts a UV-Vis full-spectrum flow detection component. The flow cell is located downstream of the filter component. The optical path, scanning wavelength range, sampling period, and spectral preprocessing method remain unchanged within the same plant natural product raw material and the same extraction grade. The calibration model is established separately according to the raw material type and extraction grade.
[0077] When establishing the mulberry leaf calibration model, samples were obtained from the first and second cycle extraction processes of no less than three batches of raw materials. The samples covered the initial, middle, and final stages of extraction, the period before and after switching the target enrichment fraction, and the cleaning and reset stage. For each extract sample, a reference sample was obtained downstream from the same detection position while the online spectrum was collected. The concentrations of chlorogenic acid and rutin were determined by high performance liquid chromatography.
[0078] High-performance liquid chromatography (HPLC) was performed using an octadecylsilane-bonded silica gel column with a gradient mobile phase consisting of an acidic aqueous solution and acetonitrile. Chlorogenic acid and rutin were confirmed by standard retention time, absorption spectrum, and spiking recovery tests, respectively. The reference value of the refractive index detection component was determined by the drying and weighing method, i.e., a quantitative extract was taken and dried at a specified temperature until the difference between two consecutive weighings was not greater than the preset weighing difference. The concentration of soluble solids was determined based on the mass of the dried residue and the sample volume.
[0079] Modeling samples are divided into calibration samples and independent validation samples. Repeated scans of the same extract should not be classified into calibration samples and independent validation samples at the same time. The model is only used for fraction distribution and extraction endpoint determination when the average relative prediction error of the independent validation results is within the allowable range and the lower limit of quantification of the model is lower than the lower limit of fraction collection of the corresponding target marker component.
[0080] The values in the table above are used to illustrate the coverage of calibration samples and the structure of independent verification. When this table is used in the formal application documents, it should be verified by the original spectra, reference chromatograms, and sample division records.
[0081] The lower limit of quantitation is constrained by both the stable quantification capability of the reference detection method and the independent validation error of the online model. It is not determined solely by the nominal sensitivity of the spectrometer. If the concentration of the target marker component is lower than the corresponding lower limit of quantitation during a certain detection period, the detection value is only used for trend observation and not for calculating extraction selectivity, breakthrough ratio, or feeding basis.
[0082] Example 4: Solvent Background, Data Validation, and Signal Reset Before each extraction stage begins, no mulberry leaf raw material is loaded into the extraction unit; only the cleaned raw material carrier basket is retained. A blank extraction solvent with the same composition as the current extraction stage flows through the extraction unit and the circulation branch. Background detection uses the same extraction liquid temperature, circulation flow rate, sampling cycle, and detection flow cell as the actual extraction.
[0083] After the temperature of the extract, the circulation flow rate, and the volume fraction of ethanol reached a stable range, detection values were continuously obtained for 12 sampling cycles. The average value of the 12 detection values was used as the background value for chlorogenic acid solvent, rutin solvent, and soluble solids solvent, respectively. The maximum positive deviation of each detection value from its corresponding average value was used as the background fluctuation. The upper limit of the allowable background range was determined by the sum of the background value and the background fluctuation.
[0084] In the actual extraction process, the corresponding solvent background value is subtracted from the target marker component detection concentration to obtain the effective detection concentration of the target marker component; when the difference is less than 0, it is recorded as 0. The effective detection concentration of soluble solids is determined in the same way. When the temperature of the extract, the circulation flow rate, or the volume fraction of ethanol exceeds the stable range, or when the effective detection concentration of soluble solids is lower than the corresponding lower limit of quantitation, the corresponding detection period is marked as an invalid period. The data of the invalid period does not control the diversion valve, does not trigger the extraction endpoint, and does not participate in the continuous judgment duration accumulation.
[0085] After the current batch of raw materials has completed all extraction stages, the extraction unit and circulation branch are rinsed with cleaning solvent. Once the chlorogenic acid, rutin, and soluble solids values all fall within their respective background allowable ranges and remain within these ranges for six consecutive sampling cycles, the control device marks the circulation branch as reset complete. The next batch of raw materials is not allowed to enter the corresponding extraction unit until the reset is complete.
[0086] Example 5: Mass flow rate, cumulative extraction volume and target enrichment fraction The mass flow rates of chlorogenic acid and rutin were determined by the effective detection concentration of the corresponding target marker component and the circulation flow rate at the same time, respectively, and were used to characterize the transmission intensity of the target marker component through the circulation branch at the detection time. The mass flow rate of the co-extracted solids was determined by the effective detection concentration of soluble solids and the circulation flow rate at the same time. The extraction selectivity was characterized by the ratio of the sum of the mass flow rates of chlorogenic acid and rutin to the mass flow rate of the co-extracted solids.
[0087] Since the circulating liquid repeatedly passes through the detection position, the mass flow rate of the target marker component cannot be directly integrated with the circulation time and used as the cumulative extraction amount. In this embodiment, the cumulative extraction amount is determined by material balance. The cumulative extraction amount includes the mass of the target marker component in the liquid phase of the current extraction unit, the mass of the target marker component actually diverted and discharged previously, and the mass of the target marker component removed by sampling and detection.
[0088] The mass of the target marker component in the liquid phase of the extraction unit is determined based on the liquid volume obtained from the liquid level detection and the current effective detection concentration of the target marker component. The mass of the target marker component discharged during each diversion period is determined based on the actual diversion volume during the diversion valve opening period and the average value of the effective detection concentration at the beginning and end of the diversion. The total flow rate of the circulation branch is not used to replace the diversion flow rate. The added solvent does not contain the target marker component, so it does not increase the cumulative extraction amount.
[0089] Divide the difference in cumulative extraction at the end of adjacent 10-minute detection time windows by the corresponding time interval to obtain the incremental recovery rate within that time window. The incremental recovery rates and their changes over three consecutive time windows together constitute the incremental recovery status.
[0090] When the extraction selectivity is not lower than the fraction collection threshold, the mass flow rate of at least one target marker component is not lower than the corresponding collection limit, and the detection concentration of another target marker component is not lower than the corresponding quantification limit, the corresponding extract is diverted to the target enrichment fraction pipeline. If the other target marker component is lower than the quantification limit, the corresponding extract is recorded and collected separately as a single-target marker component enrichment fraction and is not directly incorporated into the dual-target marker component target enrichment fraction.
[0091] When the extraction selectivity is lower than the fraction collection threshold and the incremental recovery state has not yet reached the extraction endpoint condition, the extract is returned to the extraction unit for continued circulation. When the extraction selectivity is lower than the fraction collection threshold and the current extraction stage cannot restore the target enrichment condition by continuing to circulate, the corresponding extract is introduced into the fraction to be recovered pipeline and is not mixed with the target enriched fraction.
[0092] Example 6: Two-stage cyclic extraction curve and extraction endpoint The fraction collection threshold, mass flow rate collection limit, extraction endpoint threshold, and endpoint selectivity threshold were established separately for raw material type and extraction stage. The fraction collection threshold was determined by sampling at fixed time intervals and detecting the mass of two target marker components, the mass of dried solids, and the subsequent resin adsorption performance. The extraction endpoint threshold was determined based on the relationship between the increased mass of target marker components obtained by continued extraction and the increase in co-extracted solids.
[0093] The table below lists a set of exemplary process records for 1000 grams of dried mulberry leaves. The cumulative extraction amount is calculated based on the liquid phase inventory of the extraction unit, the actual flow rate, and the sampling loss.
[0094] In the example above, the endpoint threshold for chlorogenic acid extraction in stage 1 was set to 0.010 g / min, the endpoint threshold for rutin extraction was set to 0.006 g / min, and the endpoint selectivity threshold was set to 1.0%; the endpoint threshold for chlorogenic acid extraction in stage 2 was set to 0.005 g / min, the endpoint threshold for rutin extraction was set to 0.006 g / min, and the endpoint selectivity threshold was set to 0.8%. When the incremental recovery rate of both target marker components is not higher than the corresponding threshold, the extraction selectivity is not higher than the endpoint selectivity threshold, and this condition persists for 20 minutes, the current extraction stage ends.
[0095] The endpoint determination time is no less than the response time of the online spectral detection component, the response time of the refractive detection component, the transportation time of the circulating liquid from the extraction unit to the detection position, and the maximum value of one material balance time window, thereby avoiding the premature termination of the extraction stage caused by occasional low values or pipeline transmission delays.
[0096] Example 7: Extraction of endpoint control To verify the technical contradictions addressed by the joint endpoint control, three operating modes were set up: fixed-time extraction, endpoint determination based solely on chlorogenic acid, and joint endpoint control. All three modes used the same batch of mulberry leaf raw materials, the same second-stage extraction solvent, the same temperature, and the same circulation flow rate.
[0097] While fixed-time extraction can achieve higher relative recoveries of the two target marker components, it also results in higher co-extraction solids and solvent usage. When the endpoint is determined solely based on chlorogenic acid, the continued dissolution of rutin during the second-stage extraction is not considered, leading to a decrease in the relative recovery of rutin. Combined endpoint control takes into account the incremental recovery status of chlorogenic acid and rutin, as well as the extraction selectivity of the target marker component relative to the co-extracted solids. This reduces the co-extraction load while minimizing the insufficient recovery of the other target marker component caused by premature termination of the extraction of a single target marker component.
[0098] Example 8: Control of the connection between the first and second adsorption separation columns The target enrichment fractions of dual-target marker components formed from the same batch of mulberry leaf raw materials were combined, and the ethanol volume fraction was adjusted to no more than 15% by dilution with water and recovery under reduced pressure. Before loading the sample, the concentrations of chlorogenic acid, rutin and soluble solids in the target enriched sulfur fraction were detected, and the loading flow rate was controlled within the range obtained from the dynamic adsorption verification of the resin.
[0099] The first and second adsorption separation columns are respectively filled with weakly polar macroporous adsorption resins selected through static adsorption and dynamic breakthrough tests. The resins are used after being soaked in ethanol, washed with water, and equilibrated with the sample loading solution. When loading the sample, only the first adsorption separation column is connected to the sample loading pipeline.
[0100] The penetration ratio of each target marker component is determined by the ratio of the post-column detection concentration to the pre-column detection concentration at the same time. The first penetration threshold is set to 0.10. When the penetration ratio of any target marker component reaches 0.10 and meets the requirement for 3 consecutive sampling cycles, the target marker component is determined as the first penetrating target marker component, and the second adsorption separation column is connected downstream of the first adsorption separation column within 1 sampling cycle.
[0101] During the period from the attainment of the first penetration condition to the completion of the switching valve assembly, the transition effluent discharged from the first adsorption separation column is collected separately and sent to the sample loading line of the second adsorption separation column, and is not discharged as waste liquid. After the second adsorption separation column is connected, all the effluent from the first adsorption separation column enters the second adsorption separation column.
[0102] The second penetration threshold is set to 0.05. When the penetration ratio of any target marker component in the effluent of the second adsorption separation column reaches 0.05 and meets the requirement for 3 consecutive sampling cycles, the current adsorption separation column group stops loading samples. The remaining target enriched fraction that has not been loaded is transferred to another set of adsorption separation columns that has been balanced and is not directly discharged into the fraction to be recovered.
[0103] In the example above, chlorogenic acid first reaches the first penetration threshold. Therefore, the penetration state of chlorogenic acid triggers the access of the second adsorption separation column. When the cumulative sample volume reaches 16 times the resin bed volume, the chlorogenic acid penetration ratio at the outlet of the second adsorption separation column reaches 0.052, which exceeds the second penetration threshold, and the sample loading of the current adsorption separation column group ends.
[0104] The outflow loss is determined based on the actual volume of liquid collected from the adsorption separation column outlet and the results of high performance liquid chromatography detection, and is not directly replaced by the instantaneous breakthrough ratio.
[0105] Example 9: Column elution, division and merging of basic elution fractions After sample loading, the first and second adsorption separation columns were rinsed with water until the soluble solids detection value dropped to the end limit of water washing. Then, the series connection between the two adsorption separation columns was broken, and elution was performed using ethanol aqueous solution with a volume fraction of 30% and ethanol aqueous solution with a volume fraction of 60%, respectively.
[0106] For every 0.5 times the resin bed volume of eluent, the basal elution collection container was switched once. For each basal elution, the adsorption separation column number, the volume fraction of ethanol in the eluent, the elution volume range, the mass of dried solids, the mass of chlorogenic acid, and the mass of rutin were recorded.
[0107] For each basic elution fraction, the increase in the dry basis mass fraction of chlorogenic acid relative to the mass fraction of chlorogenic acid in the dried solids of the loading solution, and the increase in the dry basis mass fraction of rutin relative to the mass fraction of rutin in the dried solids of the loading solution are compared. The basic elution fraction with a greater increase in chlorogenic acid is classified as the first elution fraction; the basic elution fraction with a greater increase in rutin is classified as the second elution fraction; the basic elution fraction whose difference in the increase between the two is within a preset boundary range is designated as the undetermined fraction.
[0108] The first and second elution fractions are divided according to the actual composition of the basic elution fraction, not mechanically based on whether the basic elution fraction comes from the first or second adsorption separation column.
[0109] After combining the first and third basic elution fractions, the dry weight mass fraction of chlorogenic acid in the first elution fraction was 8.81%, and the dry weight mass fraction of rutin was 1.29%. After combining the second and fourth basic elution fractions, the dry weight mass fraction of chlorogenic acid in the second elution fraction was 2.02%, and the dry weight mass fraction of rutin was 7.01%.
[0110] The candidate merging ratios are generated based on the mass of dried solids contained in the first elution fraction and the mass of dried solids contained in the second elution fraction. They are not generated directly according to the volumes of the two liquid fractions, but are formed in 2% mass ratio steps. The dry basis mass fractions of chlorogenic acid and rutin in the merged dried solids are determined under each candidate ratio.
[0111] In this embodiment, the batch control range for chlorogenic acid is set to 5.3%–5.7%, and the batch control range for rutin is set to 3.9%–4.3%. When the mass of the dried solids provided by the first elution fraction accounts for 51% of the mass of the combined dried solids, the dry basis mass fraction of chlorogenic acid in the combined dried solids is approximately 5.48%, and the dry basis mass fraction of rutin is approximately 4.09%. Both target marker components are within the corresponding batch control range.
[0112] When multiple candidate merging ratios meet the conditions, the deviation of each of the two target components from the median of their respective batch control ranges is calculated, and normalized according to the width of the corresponding batch control range. The candidate merging ratio with the smaller sum of the two normalized deviations is selected. If the sum of the normalized deviations of the two candidate ratios is the same, the candidate ratio that makes both target components far from the corresponding allowable upper limit is selected.
[0113] If there is no candidate merging ratio that can simultaneously meet the batch control range of two target marker components, the corresponding elution fraction is not directly used to prepare the active ingredient extract powder. Instead, the ethanol volume fraction of at least one elution fraction is adjusted to no more than 15%, and then sent to an adsorption separation column that has been equilibrated for reprocessing.
[0114] Example 10: Comparison of bulking by liquid volume and bulking by dry solids mass To illustrate the necessity of determining the merging ratio based on the mass of dried solids, three batches were merged using equal liquid volume merging and merging based on the mass of dried solids, respectively. Both merging methods used the first and second elution fractions of the same batch.
[0115] The volume fraction of ethanol and the concentration of soluble solids differ among different elution fractions. The same liquid volume does not mean the same mass of dried solids. When the fractions are combined by liquid volume, the difference in concentration will be directly transmitted to the final powder composition. When the fractions are combined by mass of dried solids, the batch-to-batch variation of the two target components is reduced.
[0116] Example 11: Concentration, Vacuum Drying, Powder Detection and Packaging The first and second eluted fractions are combined according to the determined merging ratio. The combined liquid enters a vacuum concentration unit, where ethanol is recovered under the condition that the feed liquid temperature does not exceed 60 degrees Celsius. During the concentration process, the mass of the feed liquid, the mass of the concentrate, the mass of the recovered ethanol, and the mass of the sample are recorded for material balance verification.
[0117] In this embodiment, the active ingredient extract powder is prepared by low-temperature vacuum drying to reduce the wall sticking and heat exposure that may occur when directly spray-drying polyphenol concentrate. When spray drying is used, if a food-grade drying carrier is added, the mass of the drying carrier should be included in the final dried solids mass. After drying, the dry mass fraction of the two target marker components should be re-tested, and the test results of the concentrate before drying should not be used.
[0118] Samples were taken from the upper, middle and lower parts of the dried powder, and mixed together as batch test samples. The test items included at least the powder moisture content, chlorogenic acid dry mass fraction, rutin dry mass fraction, bulk density, net content and microbiological items.
[0119] The qualified active ingredient extract powder is packaged into a composite inner sealed package that comes into direct contact with the powder, and then an outer kraft paper package is placed over the inner sealed package. Each inner sealed package is assigned a unique packaging identifier, and the extraction and separation record includes at least the mulberry leaf raw material batch, extraction unit number, start and end times of each extraction stage, target enrichment fraction range, two adsorption separation column numbers, target marker component that penetrated first, basic elution fraction range, elution fraction combination ratio, active ingredient extract powder batch, powder moisture content, dry weight fraction of the two target marker components, and net package content.
[0120] Example 12: Outer paper packaging treatment, negative pressure dust removal and ultraviolet irradiation Before the active ingredient extract powder enters the clean mixing area, the outer kraft paper packaging is first cleaned and disinfected in a non-clean unpacking area. A misting spray unit applies the disinfectant solution specified in the production site packaging cleaning and disinfection procedures to the surface of the outer kraft paper packaging. Once the continuous dripping of disinfectant no longer forms on the surface of the outer paper packaging, the outer paper packaging is removed outside the sterilization and dust removal tunnel.
[0121] When removing the outer paper packaging, separate the contact area of the outer paper packaging from the area where the inner sealed packaging is placed. After removing the inner sealed packaging, place it directly on the special carrier without contacting the outer surface of the outer paper packaging or the operating surface that supports the outer paper packaging. Inspect the seal, main body, edge sealing, powder leakage, and packaging markings of the inner sealed packaging. Any unqualified inner sealed packaging should be placed in the isolation area.
[0122] The sterilization and dust removal tunnel is equipped with three dust removal sections along the conveying direction. Each dust removal section is equipped with an air supply outlet, an air exhaust outlet, and an air baffle. The exhaust volume of the corresponding exhaust branch is greater than the air supply volume of the corresponding air supply outlet, so that the dust removal section maintains a negative pressure relative to the adjacent conveying area. The sampling end of the particulate matter detection component is set before each exhaust branch merges into the common exhaust duct.
[0123] When the dust removal section is unloaded, 12 background particulate matter detection values are continuously obtained according to the actual dust removal air volume, exhaust volume and sampling cycle. The average value of the 12 detection values is taken as the background particulate matter detection value, and the maximum positive deviation of each detection value relative to the average value is taken as the background fluctuation amount. The sum of the two is taken as the upper limit of the dust removal judgment.
[0124] After the inner sealed packaging enters the dust removal section, the particle detection value is obtained under the same sampling position, exhaust volume and sampling cycle. When the particle detection value is not higher than the dust removal judgment limit and lasts for 30 seconds, the corresponding inner sealed packaging is determined to have completed dust removal. After the previous inner sealed packaging leaves, the exhaust branch continues to operate. When the particle detection value is not higher than the dust removal judgment limit and lasts for 20 seconds, the next inner sealed packaging is allowed to enter.
[0125] The ultraviolet irradiation assembly includes a top ultraviolet irradiation unit and side ultraviolet irradiation units located on both sides of the conveying path. Starting from the completion of dust removal of the inner sealed packaging, the ultraviolet irradiation amount is accumulated based on the calibrated irradiation intensity and irradiation time received by the inner sealed packaging in the subsequent irradiation section.
[0126] When calibrating the irradiance, irradiance detection points are set at positions corresponding to the top, two sides and the edge of the inner sealed packaging. The lowest cumulative irradiance at each detection point is taken as the ultraviolet irradiance of the inner sealed packaging. Packaging samples with the same material and size as the inner sealed packaging are subjected to ultraviolet irradiation and microbial detection on the packaging surface. The lowest ultraviolet irradiance that meets the release requirements of the packaging surface is determined as the ultraviolet irradiance threshold.
[0127] In the example above, 120 millijoules per square centimeter is determined as the ultraviolet irradiance threshold for the corresponding packaging material. This threshold should be re-verified based on the actual packaging surface release requirements of the production site, the packaging material, and the ultraviolet irradiation device.
[0128] Example 13: Packaging Information Verification and Clean Material Release The inner sealed packaging that has passed the integrity check is placed in the conveyor position with a location marker. The control device associates the packaging marker, the batch number of the active ingredient extract powder, the extraction and separation record, the dust removal completion result, and the ultraviolet irradiation with the location marker.
[0129] After the inner sealed packaging arrives at the clean feeding position, the packaging label and the carrier label are read respectively. When the batch of the active ingredient extract powder corresponding to the packaging label is consistent with the batch associated with the carrier label, the dust removal completion result indicates that the dust removal has been completed, and the ultraviolet irradiation reaches the threshold, the locking state of the corresponding feeding execution component is released. If any condition is not met, the feeding execution component is kept locked and the corresponding inner sealed packaging is sent to the isolation position.
[0130] The packaging process section retains the original application's structural basis, which includes sampling before each exhaust branch converges, one dust removal section corresponding to one inner sealed package during the dust removal judgment period, cumulative ultraviolet irradiation after dust removal, and maintaining the connection between the processing record and the conveying position. The newly added extraction and separation record does not change the packaging process, but provides a data correspondence for calling the actual target marker component content of the powder in the current package at the clean feeding position.
[0131] Example 14: Determination of the dosage of dual-target marker components After release, the inner sealed packaging is removed at the clean feeding position, and the active ingredient extract powder enters the corresponding weighing device. When determining the target feeding amount, the dry mass fractions of chlorogenic acid and rutin are first converted into the actual mass fractions in the water-containing powder based on the powder moisture content. The mass fraction of the target marker component in the actual water-containing powder is determined by the corresponding dry mass fraction and the mass ratio of the dry matter in the powder.
[0132] Based on the lower and upper limits of the allowable input of chlorogenic acid specified in the formula, and the mass fraction of chlorogenic acid in the actual water-containing powder, the first allowable powder input mass range is determined; based on the lower and upper limits of the allowable input of rutin, and the mass fraction of rutin in the actual water-containing powder, the second allowable powder input mass range is determined, and the overlapping part of the two ranges is determined as the allowable input mass range.
[0133] If there is no overlap, it means that adjusting the input quality of the active ingredient extract powder in the current batch alone cannot make chlorogenic acid and rutin simultaneously meet the formulation requirements. In this case, keep the feeding execution component locked, and this batch of powder can be re-batched to form a qualified batch that complements the target marker component. If the requirements cannot be met by re-batching, the powder is redissolved and the ethanol volume fraction is adjusted before entering the re-adsorption and separation process.
[0134] When an allowable feed mass range exists, reference feed masses are determined based on the nominal feed amounts of chlorogenic acid and rutin, respectively. The target feed amount is then selected from the allowable feed mass range that minimizes the sum of the relative deviations of the two target marker components from their respective nominal feed amounts. If two identical minimum deviation candidate values exist, the smaller one is selected to reduce the risk of positive weighing deviations causing the target marker component to exceed the upper limit of the allowable feed amount.
[0135] The formulation of this embodiment specifies that the allowable amount of chlorogenic acid is 26-28 grams and the allowable amount of rutin is 20-22 grams. When the first batch is calculated separately according to the nominal amount of chlorogenic acid, the amount of rutin reaches 22.5 grams, which exceeds the upper limit of the allowable amount. When adopting the dual target allowable feed mass range and selecting 506 grams as the target feed amount, the amount of chlorogenic acid is about 26.44 grams and the amount of rutin is about 21.63 grams, both of which are within the corresponding allowable range.
[0136] Example 15: Layered feeding, final layer correction, and mixing uniformity The number of feeding layers is determined based on the target feed rate of the active ingredient extract powder, the target feed rate of the base powder, the loose packing density of the powder, the minimum stable feed rate of the feeding actuator, and the effective loading capacity of the mixing device. The active ingredient extract powder must be distributed to at least two feeding layers.
[0137] This embodiment has four feeding layers. The first feeding layer is a lower supporting base powder, the second feeding layer includes the first part of the effective ingredient extract powder, the third feeding layer includes the intermediate base powder, and the fourth feeding layer includes the second part of the effective ingredient extract powder and the upper covering base powder. The fourth feeding layer reserves space for feeding the effective ingredient extract powder for the final layer correction.
[0138] Each feeding execution component is connected to the common feeding and conveying path. After the current feeding layer completes the weighing and feeding, the weighing device stops releasing powder, but the feeding execution component and the common feeding and conveying path continue to operate. When the residual material detection component does not detect the passage of powder material for 5 consecutive sampling cycles, it is determined that the current feeding layer has been emptied, and the next feeding layer begins. The continuous detection period is not shorter than the longest conveying time required for the powder to move from the discharge end of the feeding execution component to the residual material detection component.
[0139] Before starting the fourth feeding layer, the cumulative actual amount of active ingredient extract powder from the previous feeding layers is obtained. Based on the cumulative actual amount of feed, powder moisture content, and dry mass fraction of the two target marker components, the cumulative actual amount of chlorogenic acid and rutin is determined respectively.
[0140] Based on the difference between the cumulative actual input of chlorogenic acid and its allowable input range, the quality range for replenishing chlorogenic acid in the final layer is determined; based on the difference between the cumulative actual input of rutin and its allowable input range, the quality range for replenishing rutin in the final layer is determined, and the overlapping part of the two quality ranges for replenishing rutin in the final layer is determined as the allowable corrected input quality range for the final layer.
[0141] When the lower limit of the allowable correction feed quality range for the final layer is less than 0, the lower limit is adjusted to 0. If there is no overlapping range, or if the cumulative actual input of any target marker component has exceeded the corresponding allowable input limit, the feeding execution component is locked and the mixing device is stopped. If there is an overlapping range, the final layer correction feed amount is determined from that range so that the sum of the relative deviations of the two target marker components relative to their respective nominal input amounts is small.
[0142] After the final layer correction feeding is completed and the residual material detection component confirms that the material has been emptied, the control device rechecks the cumulative actual input of chlorogenic acid and rutin. When both are within the corresponding allowable range, the mixing device is started.
[0143] After the mixing device has run for the preset mixing time, two samples are taken from the top, middle and bottom of the mixture to test for chlorogenic acid or tracer components added simultaneously with the active ingredient extract powder. If the relative standard deviation of the test results at each sampling location is not higher than 5%, the current batch is considered to have been mixed. If not, mixing continues and samples are taken again.
[0144] The relative standard deviation of the above 6 test results is less than 5%, indicating that the method of using base powder support, layered addition of active ingredient extract powder, and switching after emptying the feeding layer can meet the mixing uniformity requirements of this embodiment.
[0145] Example 16: Cleaning and Resetting, Cross-Contamination and Abnormal Handling To verify the resetting conditions of the circulation branch, after the extraction of mulberry leaves in the same extraction unit was completed, the extraction unit and circulation branch were rinsed with cleaning solvent. During the cleaning process, chlorogenic acid, rutin and soluble solids were continuously detected. If the background did not reach the allowable range, the next batch of extraction was not started.
[0146] Abnormal handling includes: when the online spectral calibration model exceeds the applicable concentration range, the corresponding fraction is transferred to the sample collection tank; when the extract temperature, circulation flow rate, or ethanol volume fraction exceeds the stable range, the extract is kept refluxed and endpoint determination is suspended; when the first adsorption separation column reaches the first breakthrough condition but the second adsorption separation column has not completed equilibrium, sample loading is stopped and the target enriched fraction is transferred to the temporary storage tank; when there is no qualified merging ratio for the eluted fraction, the re-adsorption separation process is initiated; when the packaging integrity, dust removal, or ultraviolet irradiation is unqualified, the locking of the feeding execution component must not be released; when the allowable correction feed mass range for the final layer is empty, the mixing device startup is stopped.
[0147] Example 17: Validation of the implementation method using hawthorn leaves When using hawthorn leaves, chlorogenic acid was selected as the target marker for phenolic acids, and hyperoside was selected as the target marker for flavonoids. After impurity removal, low-temperature drying, pulverization and sieving, hawthorn leaves were subjected to two-stage cyclic extraction. The first stage of cyclic extraction used an ethanol aqueous solution with a volume fraction of 30% to 40%, and the second stage of cyclic extraction used an ethanol aqueous solution with a volume fraction of 55% to 65%.
[0148] Online spectral calibration models for hawthorn leaves were established at levels 1 and 2. Exemplary calibration samples and independent validation structures are shown below.
[0149] The extraction endpoint threshold, first breakthrough threshold, second breakthrough threshold, and basic elution fraction division boundary of hawthorn leaves are re-determined based on the actual extraction curve of hawthorn leaves and the dynamic adsorption behavior of hyperoside. Only when the online detection of chlorogenic acid and hyperoside, the breakthrough order, and the column elution fraction can form a continuous control relationship according to this embodiment are the corresponding parameters used for production.
[0150] Example 18: Honeysuckle Verification Implementation Method When using honeysuckle, chlorogenic acid is selected as the target marker component for phenolic acids, and luteolin is selected as the target marker component for flavonoids. After impurity removal, low-temperature drying, pulverization and sieving, honeysuckle is subjected to two-stage cyclic extraction. Since the concentration of chlorogenic acid in honeysuckle is usually higher than that of luteolin, the online spectral calibration sample should cover the combination of high chlorogenic acid concentration and low luteolin concentration to avoid the spectral response of high concentration chlorogenic acid masking the low concentration change of luteolin.
[0151] The quantitation limit, endpoint threshold, and adsorption separation parameters of honeysuckle are not replaced by mulberry leaf parameters. When luteolin is below the corresponding quantitation limit, the corresponding detection data are not used to determine the extraction selectivity of dual-target marker components. The target marker component that actually penetrates first in the first adsorption separation column is determined by dynamic penetration detection and is not pre-specified to be chlorogenic acid or luteolin.
[0152] Example 19: Material Balance Closure and Batch Repeatability Validation To verify the data integrity during the extraction and separation process, material balance calculations were performed on the target marker components and total dried solids. The input quantity of the target marker components was based on the initial detection quantity of the raw materials, and the output quantities included the mass of the target marker components in the active ingredient extract powder, the mass of the target marker components in the sulfur to be recovered, the outlet loss of the adsorption separation column, the sampling loss, and the residual amount in the equipment cleaning solution.
[0153] When the material balance closure rate is lower than the preset range, check the sampling volume, diversion flow rate, liquid level detection, concentration measurement and cleaning fluid collection records. Batches in which the material balance has not been closed are not directly used to determine the new extraction endpoint threshold or breakthrough threshold.
[0154] Only after the main control results of three consecutive batches of mulberry leaves fall within the control range of the corresponding batch can the relevant parameters be used as production control parameters. If the origin of raw materials, harvesting season, particle size, or resin batch changes, the applicability should be reconfirmed.
[0155] Example 20: Alternative Implementation Online spectral detection components are not limited to ultraviolet-visible full-spectrum detection components; near-infrared spectral detection components can also be used. However, a calibration model should be established according to the type of raw material and extraction grade, and the prediction error and lower limit of quantitation should be confirmed through independent verification samples.
[0156] The first and second adsorption separation columns can be packed with the same macroporous adsorption resin, or different resins can be packed according to the dynamic retention capacity of the target marker component that penetrates first. When using different resins, the adsorption capacity, desorption rate and elution conditions of the two types of target marker components on the two resins should be confirmed respectively.
[0157] The basic elution fractions are not limited to switching at 0.5 times the resin bed volume; they can also be switched at a fixed time or by online detection of signal changes. However, for each basic elution fraction, records should be kept of the source adsorption separation column, eluent composition, elution volume range, dried solids mass, and mass of two target marker components.
[0158] The material conveying mechanism can adopt a belt conveyor structure, roller conveyor structure, chain conveyor structure, or carrier circulation conveyor structure. As long as it can be ensured that only one inner layer sealed package corresponds to the dust removal judgment period in any dust removal section, the form of the conveying structure does not affect the packaging correspondence in this embodiment.
[0159] The feeding actuator can be a combination of a screw feeder, a vibrating feeder, or a controlled discharge valve and a conveying component, but it should be able to switch between locked state, ready-to-start state, feeding state, and emptying operation state. The residual material detection component can be an optical detection, dielectric detection, or other non-contact detection component that can identify the powder's material state and no-load state.
[0160] It should be noted that, in this document, relational terms such as "first" and "second" are used only to distinguish one entity or operation from another, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Furthermore, the terms "comprising," "including," or any other variations thereof are intended to cover non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements includes not only those elements but also other elements not expressly listed, or elements inherent to such process, method, article, or apparatus.
[0161] Although embodiments of the invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the appended claims and their equivalents.
Claims
1. A method for ultraviolet sterilization, negative pressure dust removal, and layered feeding and mixing of sports nutrition powder in its outer packaging, characterized in that... The sports nutrition powder comprises an active ingredient extract powder and a base powder, and the method includes: Plant natural product raw materials are subjected to at least two-stage cyclic extraction. Target marker components such as phenolic acids and flavonoids and soluble solids are detected before the confluence of each cyclic branch. The target enrichment fraction and extraction endpoint are determined based on the mass flow rate, incremental recovery status and extraction selectivity of the target marker components relative to soluble solids. The target enriched fraction is first passed through the first adsorption separation column. When any target marker component reaches the breakthrough condition in the first column, the second adsorption separation column is connected downstream of it. The two columns are eluted separately, and the merging ratio is determined according to the content of the two types of target marker components in each eluted sulfur fraction. After concentration, drying and packaging, the effective ingredient extract powder is obtained. The extraction and separation records, powder moisture content, and the content of the two types of target marker components are associated with the inner sealed packaging. The inner sealed packaging is subjected to negative pressure dust removal and ultraviolet irradiation. After the dust removal is completed and the irradiation amount meets the standard, the powder feeding amount is determined together based on the allowable input amount of the two types of target marker components. The powder is fed in layers and the final layer feeding amount is adjusted according to the cumulative actual input amount. After confirming that the final layer is emptied, the powder is mixed evenly.
2. The method for ultraviolet sterilization, negative pressure dust removal, and layered feeding and mixing of sports nutrition powder in its outer packaging according to claim 1, characterized in that: The plant natural product raw material is selected from one of mulberry leaves, hawthorn leaves and honeysuckle; When the plant natural product raw material is mulberry leaf, the target marker components of phenolic acids include chlorogenic acid, and the target marker components of flavonoids include rutin or isoquercitrin. When the plant natural product raw material is hawthorn leaf, the target marker components of phenolic acids include chlorogenic acid, and the target marker components of flavonoids include hyperoside. When the plant natural product raw material is honeysuckle, the target marker components of phenolic acids include chlorogenic acid, and the target marker components of flavonoids include luteolin. The plant natural product raw materials are subjected to impurity removal, drying at a temperature not exceeding 60°C, pulverization and sieving. The particle size after pulverization is 20-60 mesh and the moisture content is not higher than 12%. The first-stage cyclic extraction uses an ethanol aqueous solution with a volume fraction of 20%-45%, and the second-stage cyclic extraction uses an ethanol aqueous solution with a volume fraction of 45%-70%.
3. The method for ultraviolet sterilization, negative pressure dust removal, and layered feeding and mixing of sports nutrition powder in its external packaging according to claim 2, characterized in that: Each circulation branch is equipped with an online spectral detection component, a refractive index detection component, a temperature detection component, and a circulation flow detection component; The online spectroscopic detection component uses calibration models established according to the type of plant natural product raw material and extraction grade to determine the detection concentration of each target marker component in the extract. The calibration model is established using target marker component standards, corresponding extract samples, and high performance liquid chromatography detection results. The refractive index value obtained by the refractive index detection component is converted into soluble solids concentration after compensation for ethanol volume fraction and extract temperature. When the concentration of the target marker component or the concentration of soluble solids is lower than the corresponding lower limit of quantitation, or when the extraction temperature or circulation flow rate exceeds the corresponding stable range, the data from the corresponding detection period are not used to determine the extraction selectivity and extraction endpoint.
4. The method for ultraviolet sterilization, negative pressure dust removal, and layered feeding and mixing of sports nutrition powder in its external packaging according to claim 3, characterized in that: Before each extraction stage begins, the extraction solvent with the same composition as the current extraction stage is flowed through the cleaned extraction unit and circulation branch to obtain the solvent background value of each target marker component and the solvent background value of soluble solids. The mass flow rate of each target marker component is determined based on the detection concentration and circulation flow rate of the target marker component after removing the solvent background. The mass flow rate of the co-extracted solids is determined based on the concentration of soluble solids after removing the solvent background and circulation flow rate. The extraction selectivity is characterized by the change in the mass flow rate of each target marker component relative to the mass flow rate of the co-extracted solids. The incremental recovery status is determined based on the changes in the cumulative extraction amount of each target marker component within adjacent detection periods; When the extraction selectivity meets the fraction collection conditions and the mass flow rate of at least one target marker component reaches the corresponding collection lower limit, the corresponding extract is split into the target enriched fraction. When the incremental recovery status of each target marker component reaches the corresponding endpoint condition, and the extraction selectivity reaches the endpoint selectivity condition and continues to reach the endpoint determination time, the current extraction stage ends. After the current batch of raw materials is extracted, the corresponding extraction unit and circulation branch are rinsed until each detection value returns to the allowable range of the corresponding solvent background and continues to do so for the signal reset time before the extraction of the next batch of raw materials begins.
5. The method for ultraviolet sterilization, negative pressure dust removal, and layered feeding and mixing of sports nutrition powder in its external packaging according to claim 4, characterized in that: Both the first and second adsorption separation columns are filled with non-polar or weakly polar macroporous adsorption resins, and the valve group switches between the single sample loading state of the first adsorption separation column and the sample loading state of the two columns in series. After the ethanol volume fraction of the target enriched fraction is adjusted to no more than 15%, it enters the first adsorption separation column. The corresponding breakthrough states are determined based on the detection concentrations of phenolic acid target marker components and flavonoid target marker components before and after the first adsorption separation column. The target marker component that first reaches the first breakthrough condition is determined as the first breakthrough marker component, and the first breakthrough condition is reached by the first breakthrough marker component as the trigger condition for the second adsorption separation column to be connected downstream of the first adsorption separation column. After the second adsorption separation column is connected, the loading ends when any target marker component in the effluent of the second adsorption separation column reaches the second breakthrough condition, or when the target enriched fraction of the current raw material batch is loaded. The second breakthrough condition is stricter than the first breakthrough condition.
6. The method for ultraviolet sterilization, negative pressure dust removal, and layered feeding and mixing of sports nutrition powder in its external packaging according to claim 5, characterized in that: After the sample loading was completed, the first adsorption separation column and the second adsorption separation column were disconnected from each other and the two columns were washed with water, eluted with low concentration ethanol, and eluted with high concentration ethanol, respectively. The first eluent fraction, in which phenolic acid target marker components are relatively enriched, and the second eluent fraction, in which flavonoid target marker components are relatively enriched, were collected separately, and the dry mass fractions of the two types of target marker components in each eluent fraction were determined. Based on the dry mass fractions of the two target marker components in the first elution fraction and the second elution sulfur fraction, a merging ratio is determined from the preset candidate merging ratios to ensure that both target marker components in the merged liquid are within the control range of the corresponding batch. When there are multiple candidate merging ratios that meet the conditions, the one with the smaller overall deviation of the two target marker components relative to their respective batch control medians is selected; when there are no candidate merging ratios that meet the conditions, at least one elution fraction is sent to the re-adsorption separation path.
7. The method for ultraviolet sterilization, negative pressure dust removal, and layered feeding and mixing of sports nutrition powder in its external packaging according to claim 6, characterized in that: After the moisture content and dry weight content of the two types of target marker components are tested, the active ingredient extract powder is packaged into an inner sealed package, and an outer paper package is placed outside the inner sealed package. Remove the outer paper packaging outside the sterilization and dust removal tunnel, check the integrity of the inner sealed packaging, and place the inner sealed packaging in the conveyor position marked with the position mark. The sterilization and dust removal tunnel is equipped with multiple dust removal sections along the conveying direction. The exhaust ports of each dust removal section are connected to the common exhaust pipe through exhaust branch lines. The particulate matter detection component samples each exhaust branch line before it merges into the common exhaust pipe. Control the conveying interval between adjacent inner sealed packages so that any dust removal section corresponds to one inner sealed package during the dust removal judgment period; When the dust removal section is in an unloaded state, the background particulate matter detection value and background fluctuation amount are obtained, and the upper limit of dust removal judgment is determined based on the background particulate matter detection value and background fluctuation amount. When the detected particulate matter value is not higher than the upper limit of the dust removal judgment and continues to reach the dust removal judgment time, the corresponding inner sealed packaging is determined to have completed dust removal.
8. The method for ultraviolet sterilization, negative pressure dust removal, and layered feeding and mixing of sports nutrition powder in its external packaging according to claim 7, characterized in that: After the first inner sealed package leaves the dust removal section, the corresponding exhaust branch continues to operate. When the particulate matter detection value returns to below the upper limit of the dust removal judgment and continues to reach the signal reset time, the second inner sealed package is allowed to enter the dust removal section. The ultraviolet irradiation assembly includes a top ultraviolet irradiation unit and side ultraviolet irradiation units located on both sides of the conveying path. Starting from the completion of dust removal of the inner sealed packaging, the subsequent ultraviolet irradiation amount is accumulated according to the calibrated irradiation intensity of each ultraviolet irradiation unit and the time it takes for the inner sealed packaging to pass through the corresponding irradiation range. The raw material batch, extraction grade, target enrichment fraction, adsorption separation column number, elution fraction merging ratio, two types of targets, dry content of marker components, moisture content, dust removal completion results, and subsequent ultraviolet irradiation are associated with the corresponding site markers. At the clean feeding position, when the material information of the inner sealed packaging is consistent with the information associated with the location identifier, dust removal has been completed, and the subsequent ultraviolet irradiation reaches the irradiation threshold, the locking state of the corresponding feeding execution component is released.
9. The method for ultraviolet sterilization, negative pressure dust removal, and layered feeding and mixing of sports nutrition powder in its external packaging according to claim 8, characterized in that: Based on the allowable dosage range of the target marker component of phenolic acids specified in the formula, the corresponding dry content, and the moisture content of the active ingredient extract powder, the first powder dosage range that meets the requirements of the target marker component of phenolic acids is determined. Based on the allowable dosage range of the target flavonoid marker components specified in the formula, the corresponding dry content, and the moisture content, the second powder dosage range that meets the requirements of the target flavonoid marker components is determined. The overlapping area between the first and second powder feedable mass ranges is defined as the allowable feedable mass range for the active ingredient extract powder. When there is no overlapping range, the corresponding feeding execution component is kept locked; when there is an overlapping range, the target feeding amount is determined from the allowable feeding quality range, and the effective ingredient extract powder is distributed to at least two feeding layers according to the target feeding amount ratio of effective ingredient extract powder to base powder.
10. The method for ultraviolet sterilization, negative pressure dust removal, and layered feeding and mixing of sports nutrition powder in its external packaging according to claim 9, characterized in that: Before the last feeding layer begins, the cumulative actual amount of the two target marker components is determined based on the cumulative actual amount of active ingredient extract powder, moisture content, and dry content of the two target marker components in the previous feeding layers. Based on the difference between the cumulative actual input of each target component and the corresponding allowable input range, the final layer replenishable input quality range that meets the requirements of each target component is determined, and the overlapping range of each final layer replenishable input quality range is determined as the final layer allowable corrective input quality range. When there is a range of allowable corrective feeding quality for the final layer, the corrective feeding amount for the final layer is determined from that range; when there is no range of allowable corrective feeding quality for the final layer, or when the cumulative actual input amount of any target marker component has exceeded the upper limit of the corresponding allowable input amount, the feeding execution component is locked and the mixing device is stopped. When the cumulative actual input of both types of target marker components is within the corresponding allowable input range, and the residual material detection component confirms that the powder material of the last feeding layer has been discharged, the mixing device is started.