Method for improving drying characteristic of schisandra chinensis extract

Abstract

The invention discloses a method for improving the drying characteristic of a Chinese magnoliavine fruit extract, which belongs to the technical field of traditional Chinese medicine preparations and comprises the following steps: adding a proper amount of auxiliary materials into a prepared Chinese magnoliavine fruit wet extract, uniformly mixing, putting into a drying oven, and carrying out vacuum drying operation to obtain the Chinese magnoliavine fruit extract after drying. The method provided by the invention solves the practical problems of low efficiency, high energy consumption, high cost and influence on the quality of the dry extract due to long-time heating in the reduced-pressure drying process of the schisandra chinensis extract. According to the method, the physicochemical property and the moisture state of the extract are improved by adding proper pharmaceutic adjuvants, the drying efficiency is improved, energy conservation and consumption reduction are achieved, and the quality of the dry extract is improved.

Description

Technical Field

[0001] The invention relates to the technical field of traditional Chinese medicine preparations, and in particular to a method for improving the drying properties of Schisandra chinensis extract. Background Art

[0002] As one of the main drying methods for Chinese medicine extracts, vacuum drying includes chamber drying, belt drying, and pulse drying. However, this technology has a series of problems in practical applications, which have become challenges that need to be urgently addressed in research and industrial production. First, the efficiency of vacuum drying is relatively low, which not only limits the expansion of production scale, but also affects the overall production progress. Secondly, due to its high energy consumption, the production cost remains high, which poses an obstacle to the sustainable development of the Chinese medicine industry. In addition, the long heating process may have an adverse effect on the quality of the dry paste, especially in terms of protecting heat-sensitive ingredients. Long-term high-temperature treatment may lead to the degradation of active ingredients, thereby reducing the quality and efficacy of the final product.

[0003] The inherent properties of Chinese medicine materials are internal factors that affect drying efficiency and quality. Chinese medicine extracts are usually highly viscous, which makes it difficult to achieve uniform heat and mass transfer during the drying process, resulting in incomplete drying or low drying efficiency. At the same time, the active ingredients in Chinese medicine extracts are very sensitive to temperature and time, and improper drying conditions may lead to reduced efficacy. Therefore, research and development of new drying technologies, or improvements to existing technologies, can improve efficiency, reduce energy consumption, reduce costs, and protect the stability of active ingredients in Chinese medicine extracts.

[0004] In view of this, the present invention is proposed. Summary of the invention

[0005] The purpose of the present invention is to improve the physical and chemical properties, moisture state, etc. of the extract by adding suitable pharmaceutical excipients, which is beneficial to improving the drying efficiency, promoting energy saving and consumption reduction in drying, and improving quality and efficiency.

[0006] In order to solve the above problems, the technical solution adopted by the present invention is:

[0007] A method for improving the drying properties of Schisandra chinensis extract comprises the following steps: adding an appropriate amount of a medicinal excipient capable of changing the drying properties of the prepared Schisandra chinensis wet extract and mixing them evenly, performing a vacuum drying operation, and obtaining the Schisandra chinensis extract after drying.

[0008] In some preferred embodiments, the relative density of the Schisandra chinensis wet extract is 1.24-1.25 g / ml.

[0009] In some preferred embodiments, the auxiliary material is maltodextrin or sodium carboxymethyl cellulose.

[0010] In some preferred embodiments, the amount of the auxiliary material is 10%-50% maltodextrin or 5%-10% sodium carboxymethyl cellulose by weight of the Schisandra chinensis wet extract.

[0011] In some preferred embodiments, the vacuum drying operation includes vacuum drying and pulsating vacuum drying.

[0012] In some preferred embodiments, the vacuum drying operation conditions are vacuum drying at 50-80°C and a vacuum upper limit of -0.09Mpa;

[0013] Or pulse vacuum drying at 50-80℃, upper vacuum limit -0.09MPa, vacuum holding time 3-5min, normal pressure holding time 1-2min.

[0014] In some preferred embodiments, during the drying process, the wet extract of Schisandra chinensis is taken out at fixed intervals for weighing to ensure that the drying is complete.

[0015] In some preferred embodiments, the water content of the Schisandra chinensis extract is less than 8%.

[0016] In some preferred embodiments, the Schisandra chinensis wet extract is prepared by crushing Schisandra chinensis slices into coarse powder suitable for extraction, adding solvent to extract three times, filtering the three times respectively and combining the filtrates, standing for 24-30 hours, and concentrating the supernatant.

[0017] In some preferred embodiments, the solvent is 75%-90% ethanol.

[0018] The present invention has the following beneficial effects:

[0019] 1. The method provided by the present invention increases the pores on the surface of the Schisandra chinensis extract, reduces the formation of the surface shell layer, reduces the water evaporation resistance, and thus accelerates the drying process of the Schisandra chinensis extract by adding appropriate pharmaceutical excipients to the Schisandra chinensis wet extract.

[0020] 2. The method provided by the present invention will affect the progress of the Maillard reaction during the vacuum drying process after adding auxiliary materials, and only reduce the content of 5-hydroxymethylfurfural during the drying process, while other components will not be affected by the drying. DETAILED DESCRIPTION

[0021] In order to make the purpose, technical scheme and advantages of the embodiments of the present invention clearer, the technical scheme in the embodiments of the present invention will be described clearly and completely below. If the specific conditions are not specified in the embodiments, they are carried out according to conventional conditions or conditions recommended by the manufacturer. If the manufacturer of the reagents or instruments used is not specified, they are all conventional products that can be purchased commercially.

[0022] In order to improve the drying rate of Schisandra chinensis extract, the present invention provides a method for improving the drying characteristics of Schisandra chinensis extract, comprising the following steps: adding an appropriate amount of pharmaceutical excipients that can change the drying characteristics of the prepared Schisandra chinensis wet extract and mixing them evenly, performing a vacuum drying operation, and obtaining the Schisandra chinensis extract after drying.

[0023] In some preferred embodiments, the relative density of the Schisandra chinensis wet extract is 1.24-1.25 g / ml.

[0024] Among them, the relative density of the extract will affect the fluidity of the extract, thereby affecting the heat transfer and water evaporation. The extract with a higher relative density may be more likely to form a crust on the surface during the drying process, hindering the evaporation of internal water. The schisandra extract with a relative density of 1.24-1.25 g / ml is selected, which has a higher relative density, which is conducive to verifying the conclusion that adding excipients in the method of the present invention will improve the drying characteristics of the extract.

[0025] In some preferred embodiments, the auxiliary material is maltodextrin or sodium carboxymethyl cellulose.

[0026] In some preferred embodiments, the amount of the auxiliary material is 10%-50% maltodextrin or 5%-10% sodium carboxymethyl cellulose by weight of the Schisandra chinensis wet extract.

[0027] Among them, maltodextrin is selected as an auxiliary material because it has high solubility and a certain degree of fusion, and can increase the viscosity of the solution, thereby improving its fluidity and dispersibility, and helping the hot air to contact the extract more evenly during the spray drying process, thereby accelerating the drying rate; sodium carboxymethyl cellulose is selected as an auxiliary material because it is a water-soluble food additive with thickening, stabilization, emulsification, and excipient effects. Sodium carboxymethyl cellulose can also form a protective layer to reduce the reabsorption of water, thereby accelerating the drying process.

[0028] In some preferred embodiments, the vacuum drying operation includes vacuum drying and pulsating vacuum drying.

[0029] Among them, vacuum drying and pulsating vacuum drying are both reduced-pressure drying. Reduced-pressure drying is currently the main drying method for Chinese medicine extracts. The Schisandra chinensis extract selected in this application has high viscosity and heat sensitivity, and has high requirements on drying efficiency and product quality. Vacuum drying and pulsating vacuum drying are both suitable for heat-sensitive materials or materials that are easily oxidized at high temperatures, so both can effectively shorten the drying time, improve product quality, and reduce energy consumption.

[0030] In some preferred embodiments, the vacuum drying operation conditions are vacuum drying at 50-80°C and a vacuum upper limit of -0.09Mpa;

[0031] Or pulse vacuum drying at 50-80℃, upper vacuum limit -0.09MPa, vacuum holding time 3-5min, normal pressure holding time 1-2min.

[0032] In some preferred embodiments, during the drying process, the wet extract of Schisandra chinensis is taken out at fixed intervals for weighing to ensure that the drying is complete.

[0033] Among them, during the drying process of Schisandra chinensis wet extract, the moisture content of the early material will drop significantly, and the moisture ratio will drop rapidly. As the drying time increases, the rate of moisture reduction in the later material will gradually slow down. Therefore, weighing the Schisandra chinensis extract at fixed intervals can effectively control the moisture content of the Schisandra chinensis extract.

[0034] In some preferred embodiments, the water content of the Schisandra chinensis extract is less than 8%.

[0035] During the drying process of Schisandra chinensis extract, the moisture content of Schisandra chinensis extract was calculated according to the weight loss formula as follows:

[0036]

[0037] Where W represents the moisture content on a dry basis (g / g), Me is the weight of the extract at the sampling point, and M0 is the weight of the extract after heating to constant weight.

[0038] In some preferred embodiments, the Schisandra chinensis wet extract is prepared by crushing Schisandra chinensis slices into coarse powder suitable for extraction, adding solvent to extract three times, filtering the three times respectively and combining the filtrates, standing for 24-30 hours, and concentrating the supernatant.

[0039] In some preferred embodiments, the solvent is 75%-90% ethanol.

[0040] The features and performance of the present invention are further described in detail below in conjunction with the embodiments.

[0041] Example 1

[0042] (1) Vacuum drying

[0043] Accurately weigh 6 portions of Schisandra chinensis wet extract of the same weight and relative density and place them in a customized metal tray to form a thickness of 3 mm. Add 10%, 30%, and 50% maltodextrin to three portions, add 5% and 10% sodium carboxymethyl cellulose to two portions, and leave the remaining portion untreated as a control. Place it in a vacuum drying oven at 80°C and -0.09MPa to dry. During the drying process, quickly take it out and weigh it at fixed intervals until the moisture content drops below 8%. Repeat the complete process 3 times for each group, and seal the dry extract in a room temperature desiccator.

[0044] (2) Pulsating vacuum drying

[0045] Accurately weigh 6 portions of Schisandra chinensis wet extract of the same weight and relative density and put them into a customized metal tray to form a thickness of 3mm. Three portions were added with 10%, 30%, and 50% maltodextrin, two portions were added with 5% and 10% sodium carboxymethyl cellulose, and the remaining portion was not treated as a control. They were placed in a pulsating vacuum drying oven at 80°C, vacuum upper limit -0.09MPa, vacuum holding time 4min, and normal pressure holding time 1min for drying. During the drying process, the extract was quickly taken out and weighed at regular intervals until the moisture content dropped below 8%. The complete process was repeated 3 times for each group, and the dry extract was sealed and stored in a room temperature desiccator.

[0046] The results of adding different auxiliary material ratios to the above-mentioned Schisandra chinensis extract and the total drying time under different drying conditions are shown in Table 1.

[0047] Table 1. Total drying time of Schisandra chinensis extract with different proportions of excipients and different drying conditions

[0048]

[0049]

[0050] The above experimental results show that under the same drying conditions, adding different proportions of auxiliary materials, the total drying time of Schisandra chinensis extract in vacuum drying and pulsating vacuum drying is shortened, and the total drying time is shortened more significantly with the increase of the proportion of auxiliary materials. The total drying time of adding 10%, 30%, and 50% maltodextrin in vacuum drying at 80℃ is shortened by 66.67%, 76.67%, and 76.67%, respectively, and the total drying time of adding 5% and 10% sodium carboxymethyl cellulose is shortened by 60%. The total drying time of adding 10%, 30%, and 50% maltodextrin in pulsating vacuum drying at 80℃ is shortened by 14.29%, 42.86%, and 57.14%, respectively, and the total drying time of adding 5% and 10% sodium carboxymethyl cellulose has no significant change.

[0051] Example 2

[0052] (1) Vacuum drying

[0053] Accurately weigh 6 portions of Schisandra chinensis wet extract of the same weight and relative density and place them in a customized metal tray to form a thickness of 3 mm. Add 10%, 30%, and 50% maltodextrin to three portions, add 5% and 10% sodium carboxymethyl cellulose to two portions, and leave the remaining portion untreated as a control. Place it in a vacuum drying oven at 80°C and -0.09MPa to dry. During the drying process, quickly take it out and weigh it at fixed intervals until the moisture content drops below 8%. Repeat the complete process 3 times for each group, and seal the dry extract in a room temperature desiccator.

[0054] Accurately weigh 0.40g of Schisandra concentrate and 0.25g of six dry pastes into a 10ml volumetric flask, add 80% methanol to the scale, weigh, and ultrasonically treat for 30 minutes. After cooling, add 80% methanol to make up the weight, and filter through a 0.22μm organic filter membrane to obtain seven test solutions. The seven test solutions were passed through a chromatographic column of ZORBAX SB-C18 (4.6×250nm) and a mobile phase of methanol-0.1% formic acid aqueous solution to detect the active ingredients of Schisandra. The test results are shown in Table 2-3.

[0055] Table 2. Determination of maltodextrin content in Schisandra chinensis extract with different proportions under vacuum drying conditions

[0056]

[0057] Different lowercase letters for the same index indicate significant differences between them (P<0.05)

[0058] Table 3. Determination of the content of carboxymethyl cellulose sodium in different proportions in Schisandra chinensis extract under vacuum drying conditions

[0059]

[0060] Different lowercase letters for the same index indicate significant differences between them (P<0.05)

[0061] Table 4. Determination of maltodextrin content in Schisandra chinensis extract with different proportions added under pulsating vacuum drying conditions

[0062]

[0063] Different lowercase letters for the same index indicate significant differences between them (P<0.05)

[0064] The above experimental results show that the content of 5-hydroxymethylfurfural in Schisandra concentrate is low, and the content of 5-hydroxymethylfurfural increases significantly after drying. Adding auxiliary materials can reduce the formation of 5-hydroxymethylfurfural during the drying process. 5-Hydroxymethylfurfural is an intermediate product of the Maillard reaction, indicating that adding auxiliary materials can reduce the occurrence of the Maillard reaction. Compared with the concentrate and the extract without adding auxiliary materials, the extract vacuum dried with auxiliary materials has no significant difference in the content of schisandra alcohol A, gomisin D, gomisin J, schisandra alcohol B, gomisin H, gomisin G, schisandra ester A, schisandra ester B, schisandra acetone, schisandra acetone, and schisandra acetone, indicating that adding auxiliary materials and vacuum drying will not change the content of these 11 components.

[0065] (2) Pulsating vacuum drying

[0066] Accurately weigh 6 portions of Schisandra chinensis wet extract of the same weight and relative density and put them into a customized metal tray to form a thickness of 3mm. Three portions were added with 10%, 30%, and 50% maltodextrin, two portions were added with 5% and 10% sodium carboxymethyl cellulose, and the remaining portion was not treated as a control. They were placed in a pulsating vacuum drying oven at 80°C, vacuum upper limit -0.09MPa, vacuum holding time 4min, and normal pressure holding time 1min for drying. During the drying process, the extract was quickly taken out and weighed at regular intervals until the moisture content dropped below 8%. The complete process was repeated 3 times for each group, and the dry extract was sealed and stored in a room temperature desiccator.

[0067] Accurately weigh 0.40g of Schisandra concentrate and 0.25g of six dry pastes into a 10ml volumetric flask, add 80% methanol to the scale, weigh, and ultrasonically treat for 30 minutes. After cooling, add 80% methanol to make up the weight, and filter through a 0.22μm organic filter membrane to obtain seven test solutions. The seven test solutions were passed through a chromatographic column of ZORBAX SB-C18 (4.6×250nm) and a mobile phase of methanol-0.1% formic acid aqueous solution to detect the active ingredients of Schisandra. The test results are shown in Table 4-5.

[0068] Table 5. Content determination of different proportions of sodium carboxymethyl cellulose in Schisandra chinensis extract under pulsating vacuum drying conditions

[0069]

[0070] Different lowercase letters for the same index indicate significant differences between them (P<0.05)

[0071] The above experimental results show that adding auxiliary materials can also reduce the formation of 5-hydroxymethylfurfural during pulsating vacuum drying. Compared with the concentrate and the extract dried with maltodextrin and sodium carboxymethyl cellulose, the extract dried with maltodextrin and sodium carboxymethyl cellulose has no significant difference in the contents of schisandrin A, gomisin D, gomisin J, schisandrin B, gomisin H, gomisin G, schisandrin ester A, schisandrin ester B, schisandrin A, schisandrin B and schisandrin C, indicating that adding auxiliary materials and pulsating vacuum drying will not change the contents of these 11 components.

[0072] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. For those skilled in the art, the present invention may have various modifications and variations. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.

Claims

1. A method for improving the drying properties of Schisandra chinensis extract, characterized in that: The following steps are involved: The prepared Schisandra chinensis wet extract is mixed with an appropriate amount of a medicinal excipient that can change the drying characteristics of the extract, and vacuum drying is performed to obtain the Schisandra chinensis extract.

2. A method for improving the drying properties of Schisandra chinensis extract according to claim 1, characterized in that: The relative density of the Schisandra chinensis wet extract is 1.24-1.25 g / ml.

3. A method for improving the drying properties of Schisandra chinensis extract according to claim 1, characterized in that: The auxiliary material is maltodextrin or sodium carboxymethyl cellulose.

4. A method for improving the drying properties of Schisandra chinensis extract according to claim 3, characterized in that: The dosage of the auxiliary material is 10%-50% maltodextrin or 5%-10% sodium carboxymethyl cellulose in weight ratio of the Schisandra chinensis wet extract.

5. A method for improving the drying properties of Schisandra chinensis extract according to claim 1, characterized in that: The vacuum drying operation includes vacuum drying and pulsating vacuum drying.

6. A method for improving the drying properties of Schisandra chinensis extract according to claim 4, characterized in that: The vacuum drying operation conditions are vacuum drying at 50-80°C and a vacuum upper limit of -0.09Mpa; Or pulse vacuum drying at 50-80℃, upper vacuum limit -0.09MPa, vacuum holding time 3-5min, normal pressure holding time 1-2min.

7. A method for improving the drying properties of Schisandra chinensis extract according to claim 1, characterized in that: During the drying process, the wet extract of Schisandra chinensis is taken out at fixed intervals and weighed to ensure that the drying is complete.

8. The method for improving the drying properties of Schisandra chinensis extract according to claim 1, characterized in that: The water content of the Schisandra chinensis extract is lower than 8%.

9. The method for improving the drying properties of Schisandra chinensis extract according to claim 1, characterized in that: The Schisandra chinensis wet extract is prepared by crushing Schisandra chinensis slices into coarse powder suitable for extraction, adding a solvent for extraction three times, filtering the three times respectively, combining the filtrates, standing for 24-30 hours, and concentrating the supernatant.

10. A method for improving the drying properties of Schisandra chinensis extract according to claim 9, characterized in that: The solvent is 75%-90% ethanol.

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