Method for simultaneously increasing the content of balisong glycosides in gastrodia elata and stabilizing it

Abstract

The present invention belongs to the technical field of processing and preparation of Chinese medicinal materials, and specifically relates to a method for simultaneously increasing the content of barisonoside components in gastrodia elata and stabilizing it. The method is: after fresh gastrodia elata is sliced, it is sequentially subjected to acetic acid-sodium acetate buffer solution soaking pretreatment, high humidity and hot air shock withering treatment and citric acid-sodium citrate buffer secondary weak acidification pretreatment, and finally dried under microwave vacuum combined conditions to obtain a dry gastrodia elata product. The gastrodia elata processing method provided by the present invention simultaneously increases the content of barisonoside A, barisonoside B and barisonoside E in gastrodia elata, and stabilizes it, and obtains gastrodia elata slices rich in barisonoside components. The contents of barisonoside A, barisonoside B and barisonoside E in the dry gastrodia elata product obtained by the processing method of the present invention are increased by 1.5-4.3 times, 2-11.4 times and 1.5-2.5 times, respectively, and can be better used as medicine and play a health care role.

Description

Technical Field

[0001] The invention belongs to the technical field of Chinese medicinal material preparation and processing, and particularly relates to a method for simultaneously increasing the content of balisong glycoside components in gastrodia elata and stabilizing the content of the components. Background Art

[0002] Gastrodia elata is the dried tuber of a perennial herbaceous plant of the genus Gastrodia in the orchid family. It is a commonly used Chinese medicine that can be used as medicine, food or health food. Gastrodia elata was first listed as a top-grade product in the Shennong's Herbal Classic under the name of "red arrow". Its "efficacy" has been highly praised by doctors and herbalists of all dynasties and the public. In 2002, Gastrodia elata was included in the "List of Items That Can Be Used as Health Foods". In 2019, Gastrodia elata was included in the pilot management of medicine and food homology, becoming one of the medicine and food homology varieties. It has been developed into a variety of products and is favored by consumers. Traditional Chinese medicine believes that Gastrodia elata has the effects of calming wind and relieving spasms, calming liver yang, and dispelling wind and unblocking meridians. Modern pharmaceutical and nutritional studies have found that Gastrodia elata has antioxidant, anti-inflammatory, analgesic, anti-epileptic, anti-anxiety and anti-depression, and improves body metabolism and sleep, which is closely related to the effective ingredients such as gastrodin, adenosine, and barreson glycosides in Gastrodia elata.

[0003] In the clinical application of gastrodin, the field faces at least the following two difficulties: 1) The absorption of gastrodin in gastrodia is affected by the transporter and is limited by absorption saturation, resulting in low bioavailability; 2) gastrodin is difficult to pass through the blood-brain barrier and has poor brain targeting. Usually, large doses are required in clinical practice to maintain effective blood drug concentrations, resulting in poor patient tolerance. Therefore, it is urgent to find an effective method to solve the problems of low bioavailability and poor patient tolerance of gastrodin. Balison glycoside compounds are formed by the condensation of gastrodin and its derivatives with citric acid at different carboxyl sites. Domestic and foreign scholars have successively isolated more than 30 Balison glycoside compounds from gastrodia, including Balison glycosides A to Z. They are all prodrugs of gastrodin, and their content in gastrodia is usually higher than that of gastrodin. Balison glycoside compounds can exert pharmacological effects by being metabolized into gastrodin, and they can also delay the half-life of gastrodin absorption and prolong the time of gastrodin activity.

[0004] Clinical studies have found that the duration of active action of balison glycosides or Gastrodia extracts is longer than that of direct administration of gastrodin, which provides new guidance for the clinical application of balison glycosides and Gastrodia extracts. Therefore, from the perspective of processing technology, the concentration and improvement of the specific balison glycosides required in Gastrodia can solve the problems of low bioavailability of gastrodin and high-dose administration in clinical practice, and at the same time provide new ways and methods for improving the quality and efficiency of Gastrodia and reducing costs and increasing efficiency.

[0005] The invention patent with publication number CN105770489B discloses a method for efficiently increasing the content of balisonoside A in Gastrodia elata, comprising the following steps: placing Gastrodia elata in a microwave device, irradiating Gastrodia elata with microwaves, and then drying at normal pressure. However, this method cannot simultaneously increase the content and stability of balisonoside A, balisonoside B, and balisonoside E in Gastrodia elata. Summary of the invention

[0006] In view of this, one of the objects of the present invention is to provide a method for simultaneously increasing the contents of balisonoside A, balisonoside B and balisonoside E in Gastrodia elata and making them in a stable state. The method of the present invention improves the content and stability of balisonoside components in Gastrodia elata through two acidification pretreatments, high humidity combined with high heat, and adjustment of pH, heating time and temperature and other conditions, thereby providing technical support for improving the quality and efficiency and reducing the cost and increasing the efficiency of Gastrodia elata.

[0007] To achieve the above object, the present invention adopts the following technical solutions:

[0008] A method for simultaneously increasing the contents of balisonoside A, balisonoside B and balisonoside E in gastrodia elata and making them in a stable state, the method comprising: sequentially subjecting fresh gastrodia elata to immersion pretreatment in an acetic acid-sodium acetate buffer solution, high-humidity hot air shock withering treatment and secondary weak acidification pretreatment with a citric acid-sodium citrate buffer solution, and finally drying under microwave vacuum combined conditions to obtain a gastrodia elata product.

[0009] The processing method of the present invention, firstly, the immersion pretreatment of acetic acid-sodium acetate buffer solution can maintain the weak acidity on the surface of fresh-cut gastrodia slices. On the one hand, the enzyme activity can be inactivated, and on the other hand, the balisong glycoside components in gastrodia can be protected in advance to prevent oxidation, degradation and structural transformation during the subsequent heating treatment process, and the ester bonds and glycosidic bonds of the balisong glycoside components can be effectively protected. Secondly, in the high-humidity hot air shock withering treatment process, high humidity combined with high temperature can synergistically promote the inactivation of α-amylase, balisong glycoside oxidase and balisong glycoside degrading enzyme in gastrodia, and at the same time can promote the effect of the acidification pretreatment in the early stage, and can also avoid the destructive effect on the balisong glycoside generating enzyme in gastrodia to a certain extent, not only can the balisong glycoside oxidase and balisong glycoside degrading enzyme be prevented from enzymolysis of the balisong glycoside components, but also can reduce the destructive effect on the balisong glycoside generating enzyme. The method of the present invention avoids the destructive effect of the traditional long-term steaming process on the balisong glycoside; at the same time, it can also avoid the loss of gastrodia active ingredients with water during the traditional steaming process. Third, the study found that the secondary weak acidification pretreatment can fully protect the ester bonds and glycosidic bonds of the barisonoside components in Gastrodia elata to prevent their degradation in the subsequent drying process. The present invention utilizes the secondary weak acidification pretreatment to effectively increase the content of barisonoside A, barisonoside B and barisonoside E in Gastrodia elata.

[0010] Furthermore, the fresh Gastrodia elata is first sliced ​​into 2mm-5mm slices.

[0011] Preferably, the pH of the acetic acid-sodium acetate buffer solution is 4.5-5.5.

[0012] Preferably, in the acetic acid-sodium acetate buffer solution immersion pretreatment, the immersion time is 30 min-45 min.

[0013] Preferably, the solid-liquid ratio of the Gastrodia elata to the acetic acid-sodium acetate buffer solution is 1:20 w / v-1:45 w / v.

[0014] Preferably, the high humidity and hot air shock killing treatment conditions are: treatment time is 1min-3min, air flow rate is 10m / s-20m / s, relative humidity is 45%-60%, and temperature is 105℃-115℃.

[0015] Furthermore, after being treated with high humidity and hot air shock, the Gastrodia elata is immediately immersed in a citric acid-sodium citrate buffer solution for soaking. Rapid cooling can prevent the ester bonds of the balisong glycoside components in the Gastrodia elata from being oxidized and degraded, and the weakly acidic environment can prevent the subsequent drying from damaging its ester bonds.

[0016] Preferably, the pH of the citric acid-sodium citrate buffer is 5.5-6.0.

[0017] Preferably, in the secondary weak acidification pretreatment, the soaking time is 10 min-30 min.

[0018] Preferably, the liquid ratio of Gastrodia elata to the citric acid-sodium citrate buffer is 1:20 w / v-1:45 w / v.

[0019] Preferably, in the vacuum-microwave combined drying of Gastrodia elata, the drying time is 2 min-10 min, the microwave power is 0.3 kW-0.5 kW, and the vacuum degree is 0.085 MPa.

[0020] Vacuuming can prevent the oxidative degradation of the balison glycosides in Gastrodia elata, and short-time microwave drying can prevent the degradation and transformation of the ester bonds and glycosidic bonds of the balison glycosides in Gastrodia elata.

[0021] The beneficial effects of the present invention are:

[0022] 1. The Gastrodia elata processing method provided by the present invention inhibits the degradation of the barisonoside components in Gastrodia elata through the interaction of pretreatment, pH, heating time and temperature, while increasing the content and stability of barisonoside A, barisonoside B and barisonoside E in Gastrodia elata, which is more conducive to the preparation of Gastrodia elata extract based on the function of barisonoside components.

[0023] 2. The process conditions provided by the present invention can increase the contents of barisonoside A, barisonoside B and barisonoside E in Gastrodia elata by 1.5-4.3 times, 2-11.4 times and 1.5-2.5 times respectively, so that the Gastrodia elata slices rich in barisonoside components obtained can be better used as medicine and play a health-care role.

[0024] 3. The preparation method of the present invention is simple and convenient, and is easy to produce, promote and apply. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] Figure 1 This is a graph showing the effects of acetic acid-sodium acetate buffer soaking conditions on the content of balisong glycosides in Gastrodia elata.

[0026] Figure 2 This is a graph showing the effect of pH of citric acid-sodium citrate buffer and phosphate buffer on the content of balisong glycosides in Gastrodia elata, wherein pH 3-6.5 is citric acid-sodium citrate buffer, and pH 7-9 is phosphate buffer.

[0027] Figure 3 This is a graph showing the effects of different processing methods on the content of balisong glycosides in Gastrodia elata. DETAILED DESCRIPTION

[0028] The technical solution of the present invention will be further described clearly and completely in conjunction with specific embodiments below. Obviously, the described embodiments are only part of the embodiments of the present invention, rather than all the embodiments. Therefore, based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative work belong to the protection scope of the present invention.

[0029] In the examples of the present invention, acetic acid and sodium acetate were purchased from Chengdu Kelon Chemical Reagent Factory; citric acid and sodium citrate were purchased from Henan Wanbang Industrial Co., Ltd.; standard products of balisonoside A, balisonoside B and balisonoside E were purchased from Shanghai Yuanye Biotechnology Co., Ltd.; other reagents for determination were purchased from Chengdu Kelon Chemical Reagent Factory.

[0030] In the embodiments of the present invention, the manufacturer / model of the high performance liquid chromatography is Shimadzu 20A; the manufacturer of the superheated steam sterilization facility is Shanghai Shen'an Instrument Factory; the manufacturer / model of the microwave vacuum dryer is Nanjing Suenrui Drying Equipment Co., Ltd. RWBZ-08S; the manufacturer / model of the hot air drying oven is Shanghai Xinmiao Instrument Equipment Factory DHG-9073BS-III.

[0031] In the embodiment of the present invention, the method for determining the balisong glycoside components in Gastrodia elata is carried out by adopting the extraction and determination method in the Chinese Pharmacopoeia 2020 edition.

[0032] Example 1

[0033] Take an appropriate amount of fresh Gastrodia elata sample, slice it with a thickness of about 3 mm, soak it in acetic acid-sodium acetate buffer solution at pH 5.5 for 35 minutes, wherein the solid-liquid ratio of Gastrodia elata to the solution is 1:25 (w / v); shock-kill it with high humidity and hot air for 1 minute; after the shock-killing with high humidity and hot air, immediately soak it in citric acid-sodium citrate buffer solution with a pH of 5.5 for 15 minutes, wherein the solid-liquid ratio of Gastrodia elata to the solution is 1:30 (w / v); finally, dry it under microwave vacuum conditions for 5 minutes, and determine the balisong in the dried Gastrodia elata.

[0034] Results: Compared with fresh Gastrodia elata (cleaning, slicing, pulping, extraction and determination of fresh Gastrodia elata), the process conditions can increase the contents of balisonoside A, balisonoside B and balisonoside E in Gastrodia elata by 4.1 times, 5.6 times and 1.9 times, respectively.

[0035] Example 2

[0036] Take an appropriate amount of fresh Gastrodia elata sample, slice it with a thickness of about 5 mm, and soak it in acetic acid-sodium acetate buffer solution at pH 5.0 for 30 minutes, wherein the solid-liquid ratio of Gastrodia elata to the solution is 1:30 (w / v); use high-humidity hot air shock to kill green for 2 minutes; after the high-humidity hot air shock to kill green, immediately place it in citric acid-sodium citrate buffer solution (pH 6.0) and soak it for 20 minutes, wherein the solid-liquid ratio of Gastrodia elata to the solution is 1:25 (w / v); finally, dry it under microwave vacuum conditions for 7 minutes, and determine the content of balisong glycoside compounds in the dried Gastrodia elata.

[0037] Results: Compared with fresh Gastrodia elata (fresh Gastrodia elata was directly washed, sliced, pulped, extracted and determined), the process conditions could increase the contents of balisonoside A, balisonoside B and balisonoside E in Gastrodia elata by 3.5 times, 10 times and 2.1 times, respectively.

[0038] Example 3

[0039] This example further studies the effect of acetic acid-sodium acetate buffer soaking conditions on the content of balisong glycosides in Gastrodia elata, and the method is as follows: five Gastrodia elata samples are taken, sliced, and soaked for 35 minutes respectively according to the conditions of no soaking, acetic acid-sodium acetate buffer at pH 3.5, 4.5, 5.5, and 6; after treatment, the samples are sterilized by high-humidity hot air shock for 1 minute; then immediately soaked in citric acid-sodium citrate buffer (pH 5.5) for 15 minutes; finally, dried under microwave vacuum conditions for 5 minutes, and the balisong glycosides in the dried Gastrodia elata are determined. Other conditions are the same as in Example 1.

[0040] Results: The immersion pretreatment in acetic acid-sodium acetate solution (pH 4.5-5.5) can inactivate enzyme activity and protect the barreson glycosides in Gastrodia elata to prevent oxidation, degradation and structural transformation during the subsequent heating process. Figure 1 As shown, the ester bonds and glycosidic bonds of the balisong glycosides can be effectively protected in the pH range of 4.5-5.5, and the content of the balisong glycosides is higher.

[0041] Example 4

[0042] This example further studies the effect of the pH of citric acid-sodium citrate buffer and phosphate buffer on the content of barrenosides in Gastrodia elata, and the method is as follows: take an appropriate amount of Gastrodia elata, clean it, slice it, and soak it in acetic acid-sodium acetate buffer at pH 5.5 for 35 minutes; after high humidity and hot air shock for 1 minute, divide it into 10 parts; according to no soaking, or soak it again for 15 minutes under the conditions of citric acid-sodium citrate buffer at pH 3, 4, 5, 5.5, 6, 6.5, and phosphate buffer at pH 7, 8, 9; finally dry it under microwave vacuum combined conditions for 5 minutes, and determine the barrenosides in the dried Gastrodia elata. Other conditions are the same as in Example 1.

[0043] Results: Figure 2 As shown in the figure, the sliced ​​Gastrodia elata treated with high humidity and hot air shock was immersed in citric acid-sodium citrate buffer (pH 5.5-6.0). It was found that the secondary weak acidification pretreatment could increase the contents of balisonoside A, balisonoside B and balisonoside E in Gastrodia elata, indicating that the secondary weak acidification pretreatment could fully protect the ester bonds and glycosidic bonds of the balisonoside components in Gastrodia elata again to prevent them from being degraded in the subsequent drying process. However, the content of balisonoside in Gastrodia elata decreased overall under strong acidic or alkaline conditions, which may be because the balisonoside components under strong acidic or alkaline conditions underwent degradation and structural transformation.

[0044] Example 5

[0045] This example further studies the effects of different processing methods on the content of balisong glycosides in Gastrodia elata, and the method is as follows:

[0046] ① Fresh Gastrodia elata: Take an appropriate amount of fresh Gastrodia elata, wash, slice, and pulp it, then extract and determine it according to the pharmacopoeia.

[0047] ② Traditional dried Gastrodia elata: Take an appropriate amount of fresh Gastrodia elata, wash and slice it, steam it in a steamer for 30 minutes, then use a hot air dryer to dry it at 60℃ for 8 hours, and then extract and measure it according to the pharmacopoeia.

[0048] ③ Vacuum-microwave drying of Gastrodia elata only: Take an appropriate amount of fresh Gastrodia elata, wash and slice it, and directly dry it under microwave-vacuum combined conditions for 5 minutes; then extract and determine it according to the pharmacopoeia;

[0049] ④ The processed Gastrodia elata of the present invention: proceed as in Example 1.

[0050] Results: Figure 3 As shown, the content of balisonoside A, balisonoside B and balisonoside E in Gastrodia elata is significantly higher than that in other processing methods by the method of the present invention. In this technical solution, pretreatment, pH, heating time and temperature inhibit the degradation of balisonoside components in Gastrodia elata through interaction, while increasing their content and stability.

[0051] The present invention takes into account the effect of processing conditions on the stability of ester bonds and glycosidic bonds of the barreson glycoside components in Gastrodia elata. Although high temperature can kill enzymes and preserve glycosides (a favorable effect), high temperature can also destroy the ester bonds and glycosidic bonds in the barreson glycoside compound molecules (an unfavorable effect). Therefore, the present invention performs weak acidification treatment on each processing step of Gastrodia elata in advance, and each processing factor synergistically plays a favorable role; although enzymes can be inhibited or even inactivated under strong acidic or alkaline conditions, the present invention has found that strong acidic or alkaline conditions can lead to the hydrolysis, degradation and structural transformation of the ester bonds of the barreson glycoside components in Gastrodia elata, and weak acid pretreatment can not only prevent the degradation of the barreson glycoside components in Gastrodia elata during high-temperature fixing and drying processes, but also weak acid conditions combined with high-temperature short-time treatment can increase the content of barreson glycoside components in Gastrodia elata, indicating that the processing process can also promote the glycosylation reaction of gastrodin and gastrodin aglycone.

Claims

1. A method for simultaneously increasing the contents of balisonoside A, balisonoside B and balisonoside E in Gastrodia elata and stabilizing them, characterized in that: The method comprises the following steps: the fresh gastrodia elata is sequentially subjected to immersion pretreatment in an acetic acid-sodium acetate buffer solution, hot and humid air shock killing treatment, and secondary weak acidification pretreatment in a citric acid-sodium citrate buffer solution, and finally dried under microwave vacuum combined conditions to obtain a gastrodia elata product; wherein, after the gastrodia elata is subjected to the hot and humid air shock killing treatment, it is immediately placed in a citric acid-sodium citrate buffer solution for immersion treatment; In the acetic acid-sodium acetate buffer solution soaking pretreatment, the pH of the acetic acid-sodium acetate buffer solution is 4.5-5.5; the solid-liquid ratio of the gastrodia elata to the acetic acid-sodium acetate buffer solution is 1:20w / v-1:45w / v; the soaking time is 30min-45min; In the high humidity hot air shock killing treatment, the killing treatment time is 1min-3min; In the secondary weak acidification pretreatment, the soaking time is 10 min-30 min; the liquid ratio of Gastrodia elata to the citric acid-sodium citrate buffer is 1:20 w / v-1:45 w / v; the pH of the citric acid-sodium citrate buffer is 5.5-6.0; In the vacuum-microwave combined drying of Gastrodia elata, the drying time is 2 min-10 min, the microwave power is 0.3 kW-0.5 kW, and the vacuum degree is 0.085 MPa.

2. The method according to claim 1, characterized in that In the high-humidity hot air impact killing treatment, the air flow rate is set to 10m / s-20m / s, the relative humidity is set to 45%-60%, and the temperature is set to 105°C-115°C.

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