Preparation quality control method of high-purity bletilla striata polysaccharide

Abstract

The invention belongs to the technical field of bletilla striata polysaccharide preparation, and provides a high-purity bletilla striata polysaccharide preparation quality control method, which comprises: constructing a raw material spectrum-polysaccharide content prediction model by using Fourier transform near infrared spectroscopy and partial least squares regression PLSR, and intelligently determining an initial material-liquid ratio based on a predicted value; in the extraction stage, the concentration is monitored in real time through an online refractometer, the ultrasonic power, the extraction time or the volume of a supplemented solvent is dynamically adjusted, and it is ensured that the concentration and the viscosity of an extracting solution are in the optimal interval; in the purification stage, the dosage of a purification reagent and the heating rate are dynamically adjusted according to the real-time concentration; in the concentration stage, according to the real-time concentration and viscosity, the vacuum degree is adjusted in a segmented mode, heating is controlled, and end point coking is prevented; according to the invention, on-line monitoring and closed-loop feedback control of key parameters in the whole process are realized, and the purity, uniformity and production stability of the product are remarkably improved.

Description

Technical Field

[0001] This invention belongs to the field of Bletilla striata polysaccharide preparation technology, specifically a quality control method for preparing high-purity Bletilla striata polysaccharide. Background Technology

[0002] Bletilla striata polysaccharide is the main active ingredient of the traditional Chinese medicine Bletilla striata. Due to its excellent hemostatic, film-forming and immunomodulatory activities, it has broad application prospects in the fields of medicine and functional food.

[0003] However, its industrial-scale preparation and quality control still face significant challenges:

[0004] First, the initial polysaccharide content of raw material Bletilla striata fluctuates greatly due to differences in origin and harvesting period. Fixed process parameters cannot be adapted to different batches of raw materials, resulting in unstable extraction efficiency and large batch-to-batch differences in product yield and quality.

[0005] Secondly, in the extraction, purification and concentration process, existing technologies mostly use pre-set fixed parameters (such as power, time and reagent dosage) for control, lacking real-time perception and dynamic control of the process status;

[0006] This can cause the concentration of the extract to deviate from the optimal range, leading to problems such as increased viscosity, decreased mass transfer efficiency, and local overheating. This not only causes the degradation of polysaccharide molecular chains and the broadening of molecular weight distribution, affecting its biological activity, but also makes it prone to coking during the concentration stage due to excessively high local concentrations, thus reducing product purity.

[0007] Therefore, there is an urgent need for a quality control method that can adapt to raw material fluctuations and accurately monitor and dynamically adjust the entire preparation process online, so as to stably obtain high-purity, high-molecular-weight, and batch-to-batch consistent Bletilla striata polysaccharide products.

[0008] Therefore, the present invention provides a quality control method for the preparation of high-purity Bletilla striata polysaccharide. Summary of the Invention

[0009] In order to overcome the shortcomings of the prior art, at least one technical problem raised in the background art is solved.

[0010] The technical solution adopted by this invention to solve its technical problem is:

[0011] In one aspect, the present invention provides a quality control method for the preparation of high-purity Bletilla striata polysaccharide, comprising:

[0012] S1: The polysaccharide content of raw material samples of Bletilla striata from different origins and harvesting periods was detected. A raw material spectrum-polysaccharide content prediction model was constructed to predict the yield of raw material samples of Bletilla striata from different origins and harvesting periods. The deviation between the predicted yield value and the detected value was verified. If the deviation is less than the deviation threshold, the material-liquid ratio was determined.

[0013] S2: During the extraction stage, obtain the real-time concentration of the extract. If the real-time concentration of the extract is less than the minimum value of the preset extraction concentration range, dynamically adjust the ultrasonic power and extraction time. If the real-time concentration of the extract is greater than the maximum value of the preset extraction concentration range, dynamically adjust the solvent volume to ensure that the viscosity of the extract is less than the preset viscosity during the extraction process.

[0014] S3: During the purification stage, a preset purification concentration range is set. If the real-time extract concentration is less than the minimum value of the preset purification concentration range, the amount of purification reagent is dynamically adjusted. If the real-time extract concentration is greater than the maximum value of the preset extraction concentration range but less than the maximum value of the preset purification concentration range, the heating rate of the purification stage is dynamically adjusted.

[0015] S4: During the concentration stage, a concentration range is preset, and the real-time extraction concentration and real-time extract viscosity are obtained. If the real-time extract viscosity is less than the viscosity threshold, the vacuum degree is dynamically adjusted according to the real-time extraction concentration to prevent coking at the concentration endpoint.

[0016] As a further innovative aspect of this invention, the specific process for constructing the raw material spectrum-polysaccharide content prediction model is as follows:

[0017] Samples of Bletilla striata from different origins and harvesting periods were collected. Spectral data of each batch of raw materials were obtained using a Fourier transform near-infrared spectrometer, and a spectral data matrix was constructed. The actual polysaccharide content of each batch of samples was determined by high-performance liquid chromatography (HPLC) as the measured value.

[0018] A raw material spectrum-polysaccharide content prediction model was constructed using partial least squares regression (PLSR). The model parameters were optimized through cross-validation to obtain the raw material spectrum-polysaccharide content prediction model.

[0019] As a further innovative aspect of the present invention, the specific process for verifying the deviation between the predicted and detected yield values ​​is as follows:

[0020] Spectral data of Bletilla striata raw material samples from different origins and harvesting periods were obtained and substituted into the raw material spectrum-polysaccharide content prediction model to predict the yield of Bletilla striata raw material samples from different origins and harvesting periods, and to verify the deviation between the predicted yield value and the detected value.

[0021] If the deviation between the predicted output and the detected output is less than the deviation threshold, then the feed-liquid ratio is determined.

[0022] If the deviation between the predicted and detected production values ​​is greater than or equal to the deviation threshold, the predicted production values ​​will be regenerated and verified.

[0023] As a further innovative aspect of this invention, the specific process for establishing the polysaccharide content-initial material-liquid ratio model is as follows:

[0024] Spectral data of Bletilla striata raw material samples from different origins and harvesting periods were obtained and substituted into the raw material spectrum-polysaccharide content prediction model to predict the yield of Bletilla striata raw material samples from different origins and harvesting periods, and to verify the deviation between the predicted yield value and the detected value.

[0025] If the deviation between the predicted output and the detected output is less than the deviation threshold, then the feed-liquid ratio is determined.

[0026] Based on the fact that the deviation between the predicted yield and the detected yield is less than the deviation threshold, a polysaccharide content-initial material-liquid ratio model is established to determine the material-liquid ratio.

[0027] Establish a polysaccharide content-initial solid-liquid ratio model: This is the production forecast.

[0028] As a further innovative aspect of the present invention, the specific process of dynamically adjusting the ultrasonic power and extraction time is as follows:

[0029] Preset extraction concentration range C extr ∈[A,B], the concentration C(t) of the extract is monitored in real time using an online refractometer;

[0030] If the real-time extract concentration C(t) < A, then adjust the ultrasonic power P and the extraction time t. extr The specific adjustment process is as follows: Where P is the adjusted ultrasonic power, P′ is the rated ultrasonic power, P″ is the power adjustment amount corresponding to a unit concentration deviation, and t extr,ext The extended extraction time is t′, where t′ represents the extension of extraction time per unit concentration deviation. This indicates taking the maximum value to ensure that the rated wave power of the ultrasound is maintained when the concentration reaches the standard. A is the minimum value of the preset extraction concentration range.

[0031] As a further innovative aspect of the present invention, the specific process of dynamically adjusting the solvent volume is as follows:

[0032] If the real-time extract concentration C(t) > B, then the solvent volume is dynamically adjusted. The specific adjustment process is as follows: Where V0 is the current extraction liquid volume, V add V′0 is the volume of solvent to be added, V″ is the preset proportional coefficient, V″ is the baseline amount of concentration difference, so as to accurately calculate the volume to be added according to the degree of concentration exceeding the standard, and B is the maximum value of the preset extraction concentration range.

[0033] As a further innovative aspect of the present invention, the specific process of dynamically adjusting the amount of purification reagent is as follows:

[0034] Preset purification concentration range C puri∈[C,D], the concentration C(t) of the extract is monitored in real time using an online refractometer;

[0035] If the real-time extract concentration C(t) < C, then the amount of purification reagent V should be dynamically adjusted. reag The increase satisfies: Among them, V reag,add V represents the increase in the amount of purification reagent. reag,base V′ is the amount of the reference reagent. reag V″ represents the percentage increase in reagent dosage corresponding to the concentration deviation per unit standard reagent dosage. reag C serves as the baseline for the concentration difference, enabling precise calculation of the reagent increase based on the degree of concentration deficiency. C represents the minimum value within the preset purification concentration range.

[0036] As a further innovative aspect of the present invention, the specific process of dynamically adjusting the heating rate during the purification stage is as follows:

[0037] If the real-time extract concentration C(t) > B and C(t) < D, then the temperature rate during the purification process should be dynamically adjusted according to the following piecewise function: Start the stirring system. B is the maximum value of the preset extraction concentration range, and D is the maximum value of the preset purification concentration range.

[0038] As a further innovative aspect of the present invention, the specific process of dynamically adjusting the vacuum degree includes:

[0039] The preset concentration range is C. conc,end ∈[E,F], obtain the real-time viscosity of the extract;

[0040] If the viscosity of the real-time extract is less than the viscosity threshold, the vacuum level is dynamically adjusted according to the real-time extract concentration. The specific dynamic adjustment process is as follows:

[0041] When the real-time extract viscosity C(t) < E, maintain a vacuum of -0.09 MPa, where E is the minimum value of the preset concentration range.

[0042] As a further innovative aspect of the present invention, the specific process of dynamically adjusting the vacuum degree also includes:

[0043] When the real-time extract viscosity E < C(t) < F, adjust the vacuum degree to -0.07 MPa;

[0044] When the real-time extract viscosity C(t) ≥ F, the heating system is turned off and active heating is stopped, so that the concentration approaches the preset concentration range, where E and F are the minimum and maximum values ​​of the preset concentration range, respectively.

[0045] On the other hand, the present invention provides a quality control system for the preparation of high-purity Bletilla striata polysaccharide, comprising:

[0046] The material-liquid ratio determination module detects the polysaccharide content of Bletilla striata raw material samples from different origins and harvesting periods, constructs a raw material spectrum-polysaccharide content prediction model, predicts the yield of Bletilla striata raw material samples from different origins and harvesting periods, verifies the deviation between the predicted yield value and the detected value, and determines the material-liquid ratio if the deviation is less than the deviation threshold.

[0047] Extraction stage control module: During the extraction stage, the real-time concentration of the extract is obtained. If the real-time concentration of the extract is less than the minimum value of the preset extraction concentration range, the ultrasonic power and extraction time are dynamically adjusted. If the real-time concentration of the extract is greater than the maximum value of the preset extraction concentration range, the solvent volume is dynamically adjusted to ensure that the viscosity of the extract is less than the preset viscosity during the extraction process.

[0048] Purification stage control module: During the purification stage, a preset purification concentration range is set. If the real-time extract concentration is less than the minimum value of the preset purification concentration range, the amount of purification reagent is dynamically adjusted. If the real-time extract concentration is greater than the maximum value of the preset extraction concentration range but less than the maximum value of the preset purification concentration range, the heating rate of the purification stage is dynamically adjusted.

[0049] Concentration stage control module: During the concentration stage, a preset concentration range is set, and the real-time extraction concentration and real-time extract viscosity are obtained. If the real-time extract viscosity is less than the viscosity threshold, the vacuum degree is dynamically adjusted according to the real-time extraction concentration to prevent coking at the concentration endpoint.

[0050] The beneficial effects of this invention are as follows:

[0051] 1. By establishing a raw material spectrum-polysaccharide content prediction model, rapid, non-destructive detection and accurate prediction of different batches of raw materials were achieved. Based on this, the optimal initial material-liquid ratio was intelligently determined, overcoming the fluctuations caused by raw material differences from the source and laying a solid foundation for subsequent stable production. By introducing online concentration and viscosity sensing and closed-loop feedback mechanisms in each stage of extraction, purification, and concentration, real-time dynamic adjustment of key process parameters such as ultrasonic power, extraction time, solvent volume, reagent dosage, heating rate, and vacuum degree was achieved. This ensured that the process parameters at each stage always matched the real-time state of the material, and the concentration and viscosity of the extract were precisely controlled within the optimal range.

[0052] 2. This method avoids increased viscosity, deteriorated mass transfer, and localized overheating caused by excessively high concentrations, significantly reducing the degradation of polysaccharide molecules and preserving their natural high molecular weight and bioactivity. Simultaneously, precise endpoint control and anti-charging strategies ensure the high purity and excellent properties of the final product. This method significantly reduces batch-to-batch variability, improves the robustness and automation of the production process, reduces energy and reagent consumption, and simultaneously ensures a balance between high yield and high quality, demonstrating promising prospects for industrial application. Attached Figure Description

[0053] The invention will now be further described with reference to the accompanying drawings.

[0054] Figure 1 This is a flowchart of the steps in the preparation and quality control method of high-purity Bletilla striata polysaccharide according to the present invention;

[0055] Figure 2 This is a system module diagram of a quality control system for the preparation of high-purity Bletilla striata polysaccharide according to the present invention. Detailed Implementation

[0056] To make the technical means, creative features, objectives and effects of this invention easier to understand, the invention will be further described below in conjunction with specific embodiments.

[0057] Example 1

[0058] like Figure 1 As shown in the embodiment of the present invention, a quality control method for preparing high-purity Bletilla striata polysaccharide includes:

[0059] S1: The polysaccharide content of raw material samples of Bletilla striata from different origins and harvesting periods was detected. A raw material spectrum-polysaccharide content prediction model was constructed to predict the yield of raw material samples of Bletilla striata from different origins and harvesting periods. The deviation between the predicted yield value and the detected value was verified. If the deviation is less than the deviation threshold, the material-liquid ratio was determined.

[0060] The polysaccharide content of raw material samples of Bletilla striata from different origins and harvesting periods was detected, and a raw material spectrum-polysaccharide content prediction model was constructed.

[0061] Samples of Bletilla striata from different origins and harvesting periods were collected. Spectral data of each batch of raw materials were obtained using a Fourier transform near-infrared spectrometer, and a spectral data matrix was constructed. The actual polysaccharide content of each batch of samples was determined by high performance liquid chromatography (HPLC) as the measured value.

[0062] A raw material spectrum-polysaccharide content prediction model was constructed using partial least squares regression (PLSR), and the model parameters were optimized through cross-validation to obtain the raw material spectrum-polysaccharide content prediction model.

[0063] For example, samples of Bletilla striata from different origins and harvesting periods were collected, and the spectral data matrix X∈R of each batch of raw materials was obtained using a Fourier transform near-infrared spectrometer (wavelength range λ∈[1000,2500]nm). n×m Where m is the number of wavelength points of the near-infrared spectrometer, X is the spectral information of all n batches of raw materials at m wavelength points, and n is the total number of batches of Bletilla striata raw materials;

[0064] The true polysaccharide content y in each batch of samples was determined by high performance liquid chromatography (HPLC). i=[y1,y2,...,y n ] T The unit is %, and y is the measured value. i Let y be the actual polysaccharide content in the i-th batch of raw materials, and T be the transpose symbol, converting the row vector into a column vector such that y i It is an n×1 column vector that stores the polysaccharide content of n batches of raw materials;

[0065] A partial least squares regression (PLSR) model was constructed to predict the spectral content of raw materials and polysaccharides. The model expression is as follows: in, Here are the predicted polysaccharide contents, x∈R m×1 Let w be the spectral data vector of a batch of raw materials, storing the spectral values ​​of the batch of raw materials at m wavelength points, which is consistent with the number of wavelength points m in matrix X, where w∈R m×1 Let b be the regression coefficient vector, and w be the intercept term. T The transpose of the regression coefficient vector w is converted into a 1×m row vector, which is used to perform the inner product operation with x, where m is the number of wavelength points of the near-infrared spectrometer.

[0066] By optimizing the model parameters through cross-validation, the number of principal components was determined to be k=8. At this time, the cross-validation error satisfies CVRE≤2%, where CVRE is the cross-validation relative error.

[0067] Yield prediction was performed on raw material samples of Bletilla striata from different origins and harvesting periods. The deviation between the predicted yield and the detected yield was verified. If the deviation was less than the deviation threshold, the material-liquid ratio was determined.

[0068] Spectral data of Bletilla striata raw material samples from different origins and harvesting periods were obtained and substituted into the raw material spectrum-polysaccharide content prediction model to predict the yield of Bletilla striata raw material samples from different origins and harvesting periods, and to verify the deviation between the predicted yield value and the detected value.

[0069] If the deviation between the predicted output and the detected output is less than the deviation threshold, then the feed-liquid ratio is determined.

[0070] If the deviation between the predicted yield and the detected yield is greater than or equal to the deviation threshold, the spectral data of the Bletilla striata raw material sample is remeasured, and the raw material spectrum-polysaccharide content prediction model is re-introduced to generate and verify the predicted yield.

[0071] Based on the fact that the deviation between the predicted yield and the detected yield is less than the deviation threshold, a polysaccharide content-initial material-liquid ratio model is established to determine the material-liquid ratio.

[0072] Establish a polysaccharide content-initial solid-liquid ratio model: This is a production forecast.

[0073] The feed-to-liquid ratio R, i.e., the raw material mass m, is determined using a piecewise function. rawWith solvent volume V solv The ratio, that is Unit: g / mL;

[0074] For example, the spectral data of the Bletilla striata raw material sample was obtained by using a Fourier transform near-infrared spectrometer, and then substituted into the raw material spectrum-polysaccharide content prediction model to obtain a yield prediction value of 19.2%.

[0075] The actual polysaccharide content of the sample was determined to be 19.5% by high performance liquid chromatography (HPLC). The calculated deviation was less than the deviation threshold because the predicted yield was 19.2%. Based on the polysaccharide content-initial material-liquid ratio model, the material-liquid ratio of this batch of Bletilla striata raw material was determined to be 1:15, that is, 1g of Bletilla striata raw material was mixed with 15mL of solvent.

[0076] Based on the feed-to-liquid ratio R = 1:15 and the predicted yield of 19.2%, the initial concentration was calculated to be 1.28%. This concentration is within the optimal range of low viscosity and high mass transfer, which can effectively avoid problems such as poor mass transfer or solvent waste caused by improper initial concentration during subsequent extraction.

[0077] It should be noted that the deviation threshold is an example selected by those skilled in the art based on historical production experience. Its purpose is only to help those skilled in the art understand the technical solution of the present invention, and it is not intended to limit the scope of protection of the present invention. The present invention is not limited to using the specific deviation threshold and material-liquid ratio mentioned above.

[0078] By combining near-infrared spectroscopy with the PLSR model, the polysaccharide content of raw materials can be predicted quickly and accurately. Based on the prediction results, the initial material-liquid ratio and initial concentration are intelligently matched using a piecewise function and concentration calculation formula. This avoids the problem of excessively high or low initial concentration from the start of preparation, providing a reasonable benchmark for subsequent staged concentration control and preventing the difficulty of subsequent processes from being increased due to initial concentration deviation.

[0079] S2: During the extraction stage, obtain the real-time concentration of the extract. If the real-time concentration of the extract is less than the minimum value of the preset extraction concentration range, dynamically adjust the ultrasonic power and extraction time. If the real-time concentration of the extract is greater than the maximum value of the preset extraction concentration range, dynamically adjust the solvent volume to ensure that the viscosity of the extract is less than the preset viscosity during the extraction process.

[0080] During the extraction stage, the real-time concentration of the extract is obtained. If the real-time concentration of the extract is less than the minimum value of the preset extraction concentration range, the ultrasonic power and extraction time are dynamically adjusted.

[0081] Preset extraction concentration range C extr ∈[A,B], the concentration C(t) of the extract is monitored in real time using an online refractometer;

[0082] If the real-time extract concentration C(t) < A, then adjust the ultrasonic power P and the extraction time t. extr The specific adjustment process is as follows: Where P is the adjusted ultrasonic power, P′ is the rated ultrasonic power, P″ is the power adjustment amount corresponding to a unit concentration deviation, and t extr,ext The extended extraction time is t′, where t′ represents the extension of extraction time per unit concentration deviation. This indicates taking the maximum value to ensure that the rated wave power of the ultrasound is maintained when the concentration reaches the standard. A is the minimum value of the preset extraction concentration range.

[0083] When the concentration of the extract C(t) < A, the solvent waste caused by premature concentration can be avoided by dynamically adjusting the ultrasonic power and extraction time.

[0084] It should be noted that the preset extraction concentration range, the power adjustment amount corresponding to the unit concentration deviation, and the extraction time extension amount corresponding to the unit concentration deviation are all reference values ​​determined by those skilled in the art based on historical production data. Due to differences in production equipment and production processes, the present invention does not limit the specific values, and the relevant values ​​can be adapted by those skilled in the art according to the actual production equipment and process requirements.

[0085] For example, the target concentration range in the extraction stage is C. extr The concentration of the extract C(t) was monitored in real time using an online refractometer within the range of [1.0%, 1.5%].

[0086] When C(t) < 1.0%, adjust the ultrasonic power P and extraction time t. extr The adjustment rules satisfy the following relationship: This adjustment prevents premature concentration and solvent waste.

[0087] If the real-time concentration of the extract is greater than the maximum value of the preset extraction concentration range, the solvent volume is dynamically adjusted to ensure that the viscosity of the extract is less than the preset viscosity during the extraction process.

[0088] Specifically, the process of adjusting the solvent volume:

[0089] If the real-time extract concentration C(t) > B, then the solvent volume is dynamically adjusted. The specific adjustment process is as follows: Where V0 is the current extraction liquid volume, V add V0′ is the volume of solvent to be added, V″ is the preset proportionality coefficient, and V″ is the baseline value of the concentration difference, used to measure the extent to which the real-time concentration C(t) exceeds the maximum value B of the preset extraction concentration range. To determine how many V″ units of concentration difference the excess part is equivalent to, and then to determine the ratio of solvent to be added, so as to accurately calculate the volume to be added based on the degree of concentration exceeding the standard, where B is the maximum value of the preset extraction concentration range;

[0090] Based on the required volume of solvent to be added, the concentration is brought back to the preset extraction concentration range. The viscosity of the extract is monitored by an online viscometer to ensure that the viscosity of the extract is less than the preset viscosity during the extraction process, thereby improving the mass transfer efficiency.

[0091] It should be noted that the preset proportional coefficient, the baseline amount of concentration difference, and the preset viscosity are all reference values ​​determined by those skilled in the art based on historical production data. Due to differences in production equipment and processes, the present invention does not limit their specific values, and the relevant values ​​can be adapted by those skilled in the art according to the actual production equipment and process requirements.

[0092] For example, when C(t) > 1.5%, the volume of solvent added V add Calculate using the following formula: After replenishment, the concentration can be brought back to the target range, and the viscosity during extraction can be monitored by an online viscometer to ensure that the viscosity is less than the preset viscosity.

[0093] S3: During the purification stage, a preset purification concentration range is set. If the real-time extract concentration is less than the minimum value of the preset purification concentration range, the amount of purification reagent is dynamically adjusted. If the real-time extract concentration is greater than the maximum value of the preset extraction concentration range but less than the maximum value of the preset purification concentration range, the heating rate of the purification stage is dynamically adjusted.

[0094] During the purification stage, a preset purification concentration range is established. If the real-time concentration of the extract is less than the minimum value of the preset purification concentration range, the amount of purification reagent is dynamically adjusted.

[0095] Preset purification concentration range C puri ∈[C,D], the concentration C(t) of the extract is monitored in real time using an online refractometer;

[0096] If the real-time extract concentration C(t) < C, then the amount of purification reagent V should be dynamically adjusted. reag The increase satisfies: Among them, V reag,add V represents the increase in the amount of purification reagent. reag,base V′ is the amount of the reference reagent. reag V″ represents the percentage increase in reagent dosage for a given concentration deviation per unit reference reagent dosage. It quantifies the proportional relationship between the additional reagent required due to concentration deviation and the reference dosage. reag This serves as a baseline for the concentration difference, used to measure the degree to which the real-time extraction concentration C(t) is insufficient relative to the minimum value C of the preset purification concentration range. Determine how many V″ the insufficient concentration is equivalent to. reag This concentration difference unit determines the multiple of additional reagent needed, enabling precise calculation of the reagent increase based on the degree of concentration deficiency, thus avoiding waste of purification reagents. C is the minimum value of the preset purification concentration range.

[0097] It should be noted that the preset purification concentration range, the reagent increase ratio corresponding to the concentration deviation under the unit reference reagent dosage, and the reference amount of the concentration difference are all reference values ​​determined by those skilled in the art based on historical production data. Due to differences in production equipment and production processes, the present invention does not limit the specific values, and the relevant values ​​can be adapted by those skilled in the art according to the actual production equipment and process requirements.

[0098] For example, the purification concentration range is C. puri ∈[2.0%, 3.0%], when C(t) < 2.0%, the amount of purification reagent V reag The increase satisfies: This formula can quantify the amount of reagent required, thus avoiding increased costs.

[0099] If the real-time extract concentration is greater than the maximum value of the preset extraction concentration range but less than the maximum value of the preset purification concentration range, the heating rate of the purification stage will be dynamically adjusted.

[0100] If the real-time extract concentration C(t) > B and C(t) < D, then the temperature rate during the purification process should be dynamically adjusted according to the following piecewise function: Simultaneously start the stirring system to ensure uniform concentration during the concentration process, without local high concentration areas, and ensure purification efficiency. B is the maximum value of the preset extraction concentration range, and D is the maximum value of the preset purification concentration range.

[0101] S4: During the concentration stage, a concentration range is preset, and the real-time extraction concentration and real-time extract viscosity are obtained. If the real-time extract viscosity is less than the viscosity threshold, the vacuum degree is dynamically adjusted according to the real-time extraction concentration to prevent coking at the concentration endpoint.

[0102] The specific process of dynamically adjusting the vacuum level is as follows:

[0103] The preset concentration range is C. conc,end ∈[E,F], obtain the real-time viscosity of the extract;

[0104] If the viscosity of the real-time extract is less than the viscosity threshold, the vacuum level is dynamically adjusted according to the real-time extract concentration. The specific dynamic adjustment process is as follows:

[0105] When the viscosity of the real-time extract C(t) < E, a vacuum of -0.09 MPa is maintained. At this vacuum, the concentration rate is moderate, which can ensure efficiency while avoiding excessive concentration increase.

[0106] When the viscosity of the real-time extract E < C(t) < F, the vacuum degree is adjusted to -0.07MPa. Reducing the vacuum degree can slow down the concentration rate and prevent the concentration from rising too rapidly near the endpoint, thus avoiding the risk of polysaccharide caramelization caused by excessively high local concentration.

[0107] When the real-time extract viscosity C(t) ≥ F, the heating system is immediately shut off and active heating is stopped. The vacuum level is finely adjusted by relying solely on the residual heat in the system, so that the concentration slowly approaches the preset concentration range. E is the minimum value of the preset concentration range and F is the maximum value of the preset concentration range.

[0108] It utilizes waste heat resources and can precisely control the final concentration, avoiding over-concentration.

[0109] It should be noted that, in this invention, those skilled in the art should understand that the preset extraction concentration range C... extr ∈[A,B], preset purification concentration range C puri ∈[C,D], preset concentration range C conc,end The concentrations in the range [E,F] are in the order A < B < C < D < E < F, with the default unit being %.

[0110] Due to differences in production equipment and processes, this invention does not limit specific values. Relevant values ​​can be adapted by those skilled in the art based on actual production equipment and process requirements.

[0111] The technical solution of this invention is as follows: The polysaccharide content of *Bletilla striata* raw material samples from different origins and harvesting periods is detected; a raw material spectrum-polysaccharide content prediction model is constructed; the yield of *Bletilla striata* raw material samples from different origins and harvesting periods is predicted; the deviation between the predicted yield and the detected yield is verified; if the deviation is less than the deviation threshold, the material-liquid ratio is determined; during the extraction stage, the real-time extract concentration is obtained; if the real-time extract concentration is less than the minimum value of the preset extraction concentration range, the ultrasonic power and extraction time are dynamically adjusted; if the real-time extract concentration is greater than the maximum value of the preset extraction concentration range, the solvent is dynamically adjusted. During the extraction process, the viscosity of the extract is kept below a preset viscosity. In the purification stage, a preset purification concentration range is established. If the real-time extract concentration is less than the minimum value of the preset purification concentration range, the amount of purification reagent is dynamically adjusted. If the real-time extract concentration is greater than the maximum value of the preset extraction concentration range but less than the maximum value of the preset purification concentration range, the heating rate of the purification stage is dynamically adjusted. In the concentration stage, a preset concentration range is established, and the real-time extraction concentration and real-time extract viscosity are obtained. If the real-time extract viscosity is less than the viscosity threshold, the vacuum level is dynamically adjusted according to the real-time extraction concentration to prevent coking at the concentration endpoint.

[0112] Example 2

[0113] like Figure 2 As shown in Example 1, this invention provides a quality control system for the preparation of high-purity Bletilla striata polysaccharide, comprising:

[0114] The material-liquid ratio determination module detects the polysaccharide content of Bletilla striata raw material samples from different origins and harvesting periods, constructs a raw material spectrum-polysaccharide content prediction model, predicts the yield of Bletilla striata raw material samples from different origins and harvesting periods, verifies the deviation between the predicted yield value and the detected value, and determines the material-liquid ratio if the deviation is less than the deviation threshold.

[0115] Extraction stage control module: During the extraction stage, the real-time concentration of the extract is obtained. If the real-time concentration of the extract is less than the minimum value of the preset extraction concentration range, the ultrasonic power and extraction time are dynamically adjusted. If the real-time concentration of the extract is greater than the maximum value of the preset extraction concentration range, the solvent volume is dynamically adjusted to ensure that the viscosity of the extract is less than the preset viscosity during the extraction process.

[0116] Purification stage control module: During the purification stage, a preset purification concentration range is set. If the real-time extract concentration is less than the minimum value of the preset purification concentration range, the amount of purification reagent is dynamically adjusted. If the real-time extract concentration is greater than the maximum value of the preset extraction concentration range but less than the maximum value of the preset purification concentration range, the heating rate of the purification stage is dynamically adjusted.

[0117] Concentration stage control module: During the concentration stage, a preset concentration range is set, and the real-time extraction concentration and real-time extract viscosity are obtained. If the real-time extract viscosity is less than the viscosity threshold, the vacuum degree is dynamically adjusted according to the real-time extraction concentration to prevent coking at the concentration endpoint.

[0118] The foregoing has shown and described the basic principles, main features, and advantages of the present invention. Those skilled in the art should understand that the present invention is not limited to the above embodiments. The embodiments and descriptions in the specification are merely illustrative of the principles of the invention. Various changes and modifications can be made to the invention without departing from its spirit and scope, and all such changes and modifications fall within the scope of the present invention as claimed. The scope of protection of the present invention is defined by the appended claims and their equivalents.

Claims

1. A quality control method for preparing high-purity Bletilla striata polysaccharide, characterized in that: include: S1: The polysaccharide content of raw material samples of Bletilla striata from different origins and harvesting periods was detected. A raw material spectrum-polysaccharide content prediction model was constructed to predict the yield of raw material samples of Bletilla striata from different origins and harvesting periods. The deviation between the predicted yield value and the detected value was verified. If the deviation is less than the deviation threshold, the material-liquid ratio was determined. S2: During the extraction stage, obtain the real-time concentration of the extract. If the real-time concentration of the extract is less than the minimum value of the preset extraction concentration range, dynamically adjust the ultrasonic power and extraction time. If the real-time concentration of the extract is greater than the maximum value of the preset extraction concentration range, dynamically adjust the solvent volume to ensure that the viscosity of the extract is less than the preset viscosity during the extraction process. S3: During the purification stage, a preset purification concentration range is set. If the real-time extract concentration is less than the minimum value of the preset purification concentration range, the amount of purification reagent is dynamically adjusted. If the real-time extract concentration is greater than the maximum value of the preset extraction concentration range but less than the maximum value of the preset purification concentration range, the heating rate of the purification stage is dynamically adjusted. S4: During the concentration stage, a concentration range is preset, and the real-time extraction concentration and real-time extract viscosity are obtained. If the real-time extract viscosity is less than the viscosity threshold, the vacuum degree is dynamically adjusted according to the real-time extraction concentration to prevent coking at the concentration endpoint.

2. The quality control method for preparing high-purity Bletilla striata polysaccharide according to claim 1, characterized in that: The specific process for constructing the raw material spectrum-polysaccharide content prediction model is as follows: Samples of Bletilla striata from different origins and harvesting periods were collected. Spectral data of each batch of raw materials were obtained using a Fourier transform near-infrared spectrometer, and a spectral data matrix was constructed. The actual polysaccharide content of each batch of samples was determined by high-performance liquid chromatography (HPLC) as the measured value. A raw material spectrum-polysaccharide content prediction model was constructed using partial least squares regression (PLSR). The model parameters were optimized through cross-validation to obtain the raw material spectrum-polysaccharide content prediction model.

3. The quality control method for preparing high-purity Bletilla striata polysaccharide according to claim 1, characterized in that: The specific process for verifying the deviation between the predicted and detected yield values ​​is as follows: Spectral data of Bletilla striata raw material samples from different origins and harvesting periods were obtained and substituted into the raw material spectrum-polysaccharide content prediction model to predict the yield of Bletilla striata raw material samples from different origins and harvesting periods, and to verify the deviation between the predicted yield value and the detected value. If the deviation between the predicted output and the detected output is less than the deviation threshold, then the feed-liquid ratio is determined. If the deviation between the predicted and detected production values ​​is greater than or equal to the deviation threshold, the predicted production values ​​will be regenerated and verified.

4. The quality control method for preparing high-purity Bletilla striata polysaccharide according to claim 3, characterized in that: The specific process for establishing the polysaccharide content-initial solid-liquid ratio model is as follows: Spectral data of Bletilla striata raw material samples from different origins and harvesting periods were obtained and substituted into the raw material spectrum-polysaccharide content prediction model to predict the yield of Bletilla striata raw material samples from different origins and harvesting periods, and to verify the deviation between the predicted yield value and the detected value. If the deviation between the predicted output and the detected output is less than the deviation threshold, then the feed-liquid ratio is determined. Based on the fact that the deviation between the predicted yield and the detected yield is less than the deviation threshold, a polysaccharide content-initial material-liquid ratio model is established to determine the material-liquid ratio. Establish a polysaccharide content-initial solid-liquid ratio model: This is the production forecast.

5. The quality control method for preparing high-purity Bletilla striata polysaccharide according to claim 1, characterized in that: The specific process of dynamically adjusting the ultrasonic power and extraction time is as follows: Preset extraction concentration range C extr ∈[A,B], the concentration C(t) of the extract is monitored in real time using an online refractometer; If the real-time extract concentration C(t) < A, then adjust the ultrasonic power P and the extraction time t. extr The specific adjustment process is as follows: Where P is the adjusted ultrasonic power, P′ is the rated ultrasonic power, P″ is the power adjustment amount corresponding to a unit concentration deviation, and t extr,ext The extended extraction time is t′, where t′ represents the extension of extraction time per unit concentration deviation. This indicates taking the maximum value to ensure that the rated wave power of the ultrasound is maintained when the concentration reaches the standard. A is the minimum value of the preset extraction concentration range.

6. The quality control method for preparing high-purity Bletilla striata polysaccharide according to claim 1, characterized in that: The specific process of dynamically adjusting the solvent volume is as follows: If the real-time extract concentration C(t) > B, then the solvent volume is dynamically adjusted. The specific adjustment process is as follows: Where V0 is the current extraction liquid volume, V add V0′ is the volume of solvent to be added, V″ is the preset proportional coefficient, V″ is the baseline amount of concentration difference, so as to accurately calculate the volume to be added according to the degree of concentration exceeding the standard, and B is the maximum value of the preset extraction concentration range.

7. The quality control method for preparing high-purity Bletilla striata polysaccharide according to claim 1, characterized in that: The specific process for dynamically adjusting the amount of purification reagent is as follows: Preset purification concentration range C puri ∈[C,D], the concentration C(t) of the extract is monitored in real time using an online refractometer; If the real-time extract concentration C(t) < C, then the amount of purification reagent V should be dynamically adjusted. reag The increase satisfies: Among them, V reag,add V represents the increase in the amount of purification reagent. reag,base V′ is the amount of the reference reagent. reag V″ represents the percentage increase in reagent dosage corresponding to the concentration deviation per unit standard reagent dosage. reag C serves as the baseline for the concentration difference, enabling precise calculation of the reagent increase based on the degree of concentration deficiency. C represents the minimum value within the preset purification concentration range.

8. The quality control method for preparing high-purity Bletilla striata polysaccharide according to claim 1, characterized in that: The specific process of dynamically adjusting the heating rate during the purification stage is as follows: If the real-time extract concentration C(t) > B and C(t) < D, then the temperature rate during the purification process should be dynamically adjusted according to the following piecewise function: Start the stirring system. B is the maximum value of the preset extraction concentration range, and D is the maximum value of the preset purification concentration range.

9. The quality control method for preparing high-purity Bletilla striata polysaccharide according to claim 1, characterized in that: The specific process of dynamically adjusting the vacuum level includes: The preset concentration range is C. conc,end ∈[E,F], obtain the real-time viscosity of the extract; If the viscosity of the real-time extract is less than the viscosity threshold, the vacuum level is dynamically adjusted according to the real-time extract concentration. The specific dynamic adjustment process is as follows: When the real-time extract viscosity C(t) < E, maintain a vacuum of -0.09 MPa, where E is the minimum value of the preset concentration range.

10. The quality control method for preparing high-purity Bletilla striata polysaccharide according to claim 9, characterized in that: The specific process of dynamically adjusting the vacuum level also includes: When the real-time extract viscosity E < C(t) < F, adjust the vacuum degree to -0.07 MPa; When the real-time extract viscosity C(t) ≥ F, the heating system is turned off and active heating is stopped, so that the concentration approaches the preset concentration range, where E and F are the minimum and maximum values ​​of the preset concentration range, respectively.

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