Preparation method of salted cistanche wine product

Abstract

The invention belongs to the technical field of traditional Chinese medicine processing, and particularly relates to a preparation method of a salted cistanche wine product. The invention relates to a preparation method of a salted cistanche wine product. According to the method, echinacoside, cistanoside A, verbascoside, isoacteoside, 2 '-acetyl verbascoside and extract content are selected as evaluation indexes, a high performance liquid chromatography (HPLC) method is adopted to detect the evaluation indexes in cistanche deserticola crude products and decoction pieces washed with wine to remove salt, and a response surface test design method is adopted to determine the content of echinacoside, cistanoside A, verbascoside, isoacteoside, 2'-acetyl verbascoside and extract. Evaluating and optimizing investigation factors of the cistanche wine washing process through a comprehensive scoring method, and obtaining an optimal preparation process of the wine-washed cistanche.

Description

Technical Field

[0001] The invention relates to the technical field of Chinese medicine processing, and specifically relates to a method for preparing a salt-raw Cistanche deserticola wine product. Background Art

[0002] According to the records of Compendium of Materia Medica of various dynasties, the original plants of Cistanche deserticola are C. deserticola and C. salsa (CAMey.) G. Beck. Among them, the Cistanche harvested in spring is called light dayun, and the one harvested in autumn and soaked in salt lake is called salt dayun. During the processing of salt dayun, it is required to rinse it until it is light. According to the records in the herbal classics "Pharmaceutical Huayi", "soak with wine to remove the floating scales, clean out the saltiness, split the center, brush off a layer of white film, and then cook with white wine until it is soft"; according to the records in "Depei Materia Medica", "bleach it very lightly, steam it for half a day, or roast it with butter"; according to the records in "Ben Jing Feng Yuan", "wash it with wine, remove the scales and rot, slice it and bake it"; according to "Ben Cao Tu Jing", "Westerners often eat it as food. Scrape off the scales, wash it with wine, remove the black juice, cut it thinly, and make a soup with taro and mutton. It is very delicious and beneficial to people, and eating it is better than taking tonic medicine"; according to "Ben Cao Yan Yi", "wash it with wine, remove the black juice, and make a soup. After the black juice is gone, the smell is gone. However, only the young ones can be used to make a soup, the old ones are bitter"; and the classic recipe "Jichuan Jian" from "Jingyue Complete Works" by Zhang Jingyue in the Ming Dynasty records that the slices of Cistanche deserticola are washed with wine to remove the saltiness. However, modern processing specifications are not included, and the quality of its decoction pieces lacks corresponding specifications, making it difficult to ensure the stability and controllability of the processed products. Therefore, this field needs to use modern technology and analytical technology to develop a processing method for salt-raw Cistanche deserticola wine washing.

[0003] At present, the dried fleshy stems with scale leaves of Cistanche deserticola Y.C.Ma or Cistanche tubulosa (Schenk) Wight, which are plants of the Orobanchaceae family, are usually used to prepare Cistanche deserticola slices. The traditional processing method is to take raw Cistanche deserticola, add rice wine, put it in a suitable container, seal it, heat it with steam or steam, and stew it thoroughly, or stew it until the rice wine is completely absorbed, cool it, take it out, dry it to 60%, slice it, and dry it. However, the modern processing of Cistanche deserticola slices washed with wine is not recorded, and it is not clear whether there is a difference in clinical efficacy between the Cistanche deserticola slices washed with wine and the slices steamed or stewed with wine in the ancient recipe "Jichuan Jian". Summary of the invention

[0004] Therefore, the technical problem to be solved by the present invention is to provide a method for preparing a salt-raw Cistanche deserticola wine product.

[0005] In order to solve the above technical problems, the preparation method of a salt-raw Cistanche deserticola wine product of the present invention comprises the steps of spraying rice wine on the surface of the salt-raw Cistanche deserticola raw product for wine soaking;

[0006] The mass ratio of the raw salt-cistanche deserticola to rice wine is 2:1-1:2;

[0007] The wine soaking time is 5-45 minutes, and the wine soaking times are 2-4 times.

[0008] Specifically, in the preparation method of the salt-raw Cistanche deserticola wine product, the mass ratio of the salt-raw Cistanche deserticola product to rice wine is 50g:99g, the wine immersion time is 6 minutes, and the wine immersion times are 2 times.

[0009] Specifically, the method for preparing the salt-raw Cistanche deserticola wine product further comprises the step of drying the raw salt-raw Cistanche deserticola product;

[0010] Preferably, the temperature of the drying step is 55-60°C.

[0011] Specifically, the method for preparing the salt-raw Cistanche deserticola wine product also includes the step of constructing a comprehensive scoring model for the salt-raw Cistanche deserticola wine product, and the step of evaluating the quality of the salt-raw Cistanche deserticola wine product based on the comprehensive scoring model.

[0012] Specifically, the preparation method of the salt-raw Cistanche deserticola wine product, the comprehensive scoring model of the salt-raw Cistanche deserticola wine product is: OD = 0.340 × D X1 +0.192×D X2 +0.058×D X3 +0.145×D X4 +0.079×D X5 +0.186×D X6 ;in,

[0013] D X1 is the content of echinacoside, D X2 is the verbascoside content, D X3 is the content of isoverbascoside, D X4 is the content of 2'-acetyl verbascoside, D X5 is the content of Cistanche deserticola glycoside A, D X6 It is the extract content of the salt-raw Cistanche deserticola wine product.

[0014] Specifically, the method for preparing the salt-raw Cistanche deserticola wine product further comprises the step of determining the content of the salt-raw Cistanche deserticola wine product extract and the effective ingredients of the salt-raw Cistanche deserticola wine product;

[0015] The active ingredients include echinacoside, verbascoside, isovalascoside, 2'-acetylverbascoside, cistancheside A

[0016] The method for determining the effective component content of the salt-raw Cistanche deserticola wine product comprises high performance liquid chromatography.

[0017] Specifically, the preparation method of the salt-raw Cistanche deserticola wine product, the chromatographic conditions of the high performance liquid chromatography include: using octadecylsilane bonded silica gel as a filler, acetonitrile as a mobile phase A, and 0.5% acetic acid aqueous solution as a mobile phase B, and performing gradient elution according to the following procedure:

[0018] 0-6min, A: 10% → 15%, B: 90% → 85%;

[0019] 6-10min, A: 15% → 18%, B: 85% → 82%;

[0020] 10-15min, A: 18%, B: 82%;

[0021] 15-25min, A: 18%→20%, B: 82%→80%;

[0022] 25-35min, A: 20% → 23%, B: 80% → 77%;

[0023] 35-37min, A: 23%→10%, B: 77%→90%.

[0024] Specifically, in the method for preparing the salt-raw Cistanche deserticola wine product, the chromatographic conditions of the high performance liquid chromatography also include: flow rate 1 min / mL, column temperature 30°C, injection volume 10 μL, and detection wavelength 330 nm.

[0025] Specifically, the preparation method of the salt-raw Cistanche wine product and the preparation method of the extract of the salt-raw Cistanche wine product include: taking the salt-raw Cistanche wine product and adding 50v / v% ethanol solution for cold soaking, filtering with a drying filter, and taking the filtrate for evaporation and weighing.

[0026] Specifically, the method for preparing the salt-raw Cistanche deserticola wine product further comprises the step of preparing a test solution of the salt-raw Cistanche deserticola wine product;

[0027] The preparation steps of the test solution include: accurately weighing the salt-raw Cistanche deserticola wine product, adding 50% methanol to soak, adding 50% methanol to make up the weight after ultrasonic treatment, centrifuging and filtering, and collecting the filtrate to obtain the test solution.

[0028] The preparation method of the salt-raw Cistanche deserticola wine product of the present invention, on the basis of systematically combing the chemical components of the wine-washed Cistanche deserticola, selects echinacoside, cistancheside A, verbascoside, isovalascoside, 2'-acetylverbascoside and extract content as evaluation indicators, adopts high performance liquid chromatography (HPLC) to detect the evaluation indicators in the raw Cistanche deserticola and the wine-washed desalted slices, adopts response surface experimental design method, evaluates and optimizes the investigation factors of the wine-washing process of Cistanche deserticola by comprehensive scoring method: that is, the ratio of decoction slices / yellow wine, wine immersion time and wine washing times, and obtains the best preparation process of wine-washed Cistanche deserticola. The present invention finally screens out the optimal processing technology and parameters of the salt-raw Cistanche deserticola wine product, and provides a scientific basis for the formulation of the processing technology standard of wine-washed Cistanche deserticola.

[0029] The method for preparing the salt-raw Cistanche deserticola wine product of the present invention selects the salt-raw Cistanche deserticola raw product, examines the optimal types of processing with three types of wine, namely, yellow wine, rice wine and white wine, and examines the ratio of auxiliary wine to the slices of 2:1, 1:1, 1:1.5, 1:2, 1:3, and selects the optimal wine dosage range, sprays the wine evenly on the slices, examines the wine immersion time of 5, 15, 30, 45, 60, 90 minutes, and after determining the optimal wine immersion time range, examines the wine immersion times of 2, 3, 4, 5, and 6 times. The method for preparing the salt-raw Cistanche deserticola wine product of the present invention preferably uses the auxiliary material yellow wine, with a yellow wine and slice ratio of 2:1-1:2, sprays the wine evenly on the slices, the wine immersion time is 5-45 minutes, and the wine immersion times are 2-4 times. The preparation method of the salt-raw Cistanche deserticola wine product of the present invention is further optimized by using response surface experiment combined with AHP-CRITIC method comprehensive scoring, and the auxiliary material decoction piece / yellow wine ratio is 50g / 99g, the wine immersion time is 6min, and the wine washing times is 2 times.

[0030] The preparation method of the salt-raw Cistanche deserticola wine product of the present invention comprises the following steps: accurately analyzing the components of the salt-raw Cistanche deserticola, selecting echinacoside, cistancheside A, verbascoside, isoverbosaside, 2'-acetylverbosaside and extract content as evaluation indexes of the wine-washed Cistanche deserticola; and using high performance liquid chromatography to measure the content of the evaluation indexes in the wine-washed Cistanche deserticola prepared by different preparation methods; and comparing the correlation of various evaluation indexes in the wine-washed Cistanche deserticola obtained by different methods by AHP method, CRITIC method and AHP-CRITIC method, and selecting the AHP-CRITIC method whose information of the reaction is not superimposed to determine the index weight and calculate the comprehensive score. The preparation method of the wine-washed Cistanche deserticola with a high comprehensive score is selected as the optimized preparation method of the wine-washed Cistanche deserticola.

[0031] The preparation method of the salt-raw Cistanche deserticola wine product of the present invention, the comprehensive evaluation refers to comparing the response surface test content determination results and extract content results of the wine Cistanche deserticola obtained by different preparation methods through a multi-index comprehensive scoring method, and the data are first standardized during the scoring process, and the echinacoside content is D X1 , the content of verbascoside is D X2 , the content of iso-verbascoside is D X3 , 2'-acetyl verbascoside content is D X4 , the content of Cistanche deserticola A is D X5 , the extract content is D X6 The weight coefficient of echinacoside was set to 0.340, the weight coefficient of verbascoside was 0.192, the weight coefficient of isovalascoside was 0.058, the weight coefficient of 2'-acetylverbascoside was 0.145, the weight coefficient of cistancheside A was 0.079, and the weight coefficient of extract was 0.186. The comprehensive value was used for statistical analysis, and the comprehensive scoring formula was OD = 0.340 × D X1 +0.192×D X2 +0.058×D X3 +0.145×D X4 +0.079×D X5 +0.186×D X6 .

[0032] The preparation method of the salt-raw Cistanche deserticola wine product of the present invention, the total amount of echinacoside and verbascoside in the prepared wine-washed salted Cistanche deserticola slices is not less than 1.47%, which is much higher than the total amount of echinacoside and verbascoside in the wine-washed Cistanche deserticola slices in the 2020 edition of the Chinese Pharmacopoeia. BRIEF DESCRIPTION OF THE DRAWINGS

[0033] In order to make the content of the present invention more clearly understood, the present invention is further described in detail below according to specific embodiments of the present invention in conjunction with the accompanying drawings, wherein:

[0034] Figure 1 It is the HPLC chart of the mixed reference solution in Example 2; wherein, 1: echinacoside, 2: cistancheside A, 3: verbascoside, 4: isovalascoside, 5: 2'-acetylverbascoside;

[0035] Figure 2 The HPLC chart of the wine-washed salted Cistanche slices in Example 2; wherein, 1: echinacoside, 2: cistancheside A, 3: verbascoside, 4: isovalascoside, 5: 2'-acetylverbascoside;

[0036] Figure 3 It is a three-dimensional space surface diagram of the salt-raw Cistanche deserticola wine product described in Example 5;

[0037] Figure 4 This is a contour map of the salt-raw Cistanche deserticola wine product described in Example 5. DETAILED DESCRIPTION

[0038] The preferred embodiments of the present invention are described below in conjunction with the accompanying drawings. It should be understood that the preferred embodiments described herein are only used to illustrate and explain the present invention, and are not used to limit the present invention.

[0039] In the following embodiments of the present invention, the experimental equipment involved is as follows:

[0040] Agilent 1220infintyⅡ liquid chromatograph (Agilent, USA);

[0041] AE240 1 / 100,000 electronic balance (Mettler-Toledo, Switzerland);

[0042] CP214 1 / 10,000 electronic analytical balance (Ohaus Instruments Shanghai Co., Ltd.);

[0043] Manual slicer (Guangdong Shandao Kitchenware Co., Ltd.);

[0044] 2-liang high-speed Chinese medicine pulverizer (Ruian Yongli Pharmaceutical Machinery Co., Ltd.);

[0045] GZX-9076MBE electric heating blast drying oven (Shanghai Boxun Industrial Co., Ltd. Medical Equipment Factory);

[0046] KQ-600DE CNC ultrasonic cleaner (Kunshan Ultrasonic Instrument Co., Ltd.);

[0047] MZ-ZGC322301 Midea electric steamer (Guangdong Midea Household Electrical Appliance Manufacturing Co., Ltd.);

[0048] Dynamica velocity 18R pro tabletop centrifuge (Dynamica, UK);

[0049] SX-4-10 box-type resistance furnace (Tianjin Tiantai Instrument Co., Ltd.).

[0050] In the following embodiments of the present invention, the experimental reagents involved are as follows:

[0051] Echinacoside (batch number CHB201212), verbascoside (batch number CHB211109), isovalascoside (batch number CHB210105), 2'-acetylverbascoside (batch number CHB201126), tubuloside A (batch number HB201219), purity ≥98%, cistancheside A (batch number CHB201203, purity ≥95%) (Chengdu Kroma Biotechnology Co., Ltd.);

[0052] Shazhou Youhuang (Jiangsu Zhangjiagang Brewing Co., Ltd., batch number: 20230313, total sugar in glucose: 15.1-40.0 g / l), original high-grade glutinous rice wine (Nanchang High-tech Industrial Development Zone Maqiu Fucha Rice Wine Shop, batch number: 20230202, alcohol content: 25% vol), Red Star Erguotou (Beijing Red Star Co., Ltd., batch number: 20221231, alcohol content: 56% vol), water is ultrapure water, acetonitrile and acetic acid are chromatographic grade, and other reagents are analytical grade;

[0053] The original medicinal material of Cistanche deserticola was purchased from Jiangxi Jizhongtang Health Technology Co., Ltd., batch number RCR-AYQ-YC-202201, and was identified as the dried fleshy stem with scaly leaves of Cistanche salsa (CA Mei.) G. Beck.

[0054] Example 1 Detection method construction

[0055] Evaluation index screening

[0056] According to the literature research on the chemical composition of Cistanche deserticola, echinacoside has the effects of anti-cerebral ischemia, liver protection and anti-inflammatory, verbascoside has the effects of anti-hypoxic myocardial damage and anti-vascular dementia, iso-verbascoside has the effect of improving renal damage, 2'-acetyl verbascoside has the effect of anti-osteoclast formation, and Cistanche glycoside A has the effects of regulating osteoblast differentiation, mineralization, anti-inflammatory and antioxidant effects. At the same time, the pre-experiment of the wine washing and salt removal processing process found that the contents of echinacoside, verbascoside and 2'-acetyl verbascoside in Cistanche deserticola changed significantly after wine processing, and the extract content is a major indicator for the evaluation of medicinal pieces. Therefore, this embodiment selects echinacoside, Cistanche glycoside A, verbascoside, iso-verbascoside, 2'-acetyl verbascoside and extract content as evaluation indicators.

[0057] Chromatographic conditions

[0058] YMC-Pack ODS-A column (4.6 mm × 250 mm, 5 μm);

[0059] Mobile phase: acetonitrile (A)-0.5% acetic acid aqueous solution (B);

[0060] Perform gradient elution as follows:

[0061] 0-6min, A: 10% → 15%, B: 90% → 85%;

[0062] 6-10min, A: 15% → 18%, B: 85% → 82%;

[0063] 10-15min, A: 18%, B: 82%;

[0064] 15-25min, A: 18%→20%, B: 82%→80%;

[0065] 25-35min, A: 20% → 23%, B: 80% → 77%;

[0066] 35-37min, A: 23% → 10%, B: 77% → 90%;

[0067] The flow rate was 1 min / mL, the column temperature was 30°C, the injection volume was 10 μL, and the detection wavelength was 330 nm; the theoretical plate number of echinacoside was >3000, and the chromatographic peak had good symmetry.

[0068] Preparation of mixed reference solution

[0069] Take appropriate amount of echinacoside, cistancheside A, verbascoside, isovalascoside and 2'-acetylverbascoside reference substances, weigh accurately, add 50% methanol to make a mother solution containing 0.28 mg of each per 1 mL, dilute to the corresponding concentration by the doubling dilution method, and prepare the standard curve solution.

[0070] Preparation of test solution for salt-raw Cistanche deserticola wine product

[0071] According to the preparation method of the test solution under the item of Cistanche content determination in the "Chinese Pharmacopoeia", take about 1.00g of salt-raw Cistanche wine product powder (passed through No. 4 sieve), accurately weigh it, put it in a 100mL brown volumetric flask, accurately add 50mL of 50% methanol, seal it, shake it well, weigh it, soak it for 30 minutes, ultrasonically treat it for 40 minutes (power 250W, frequency 35kHz), cool it, weigh it again, add 50% methanol to make up for the lost weight, shake it well, let it stand, take 2mL of the liquid, 5000rpm, 10℃, centrifuge it for 10min, take the supernatant and filter it through a 0.22μm filter membrane, and take the filtrate to obtain it.

[0072] Preparation of leachate samples

[0073] According to the determination method of Cistanche extract in the Chinese Pharmacopoeia (2020 edition), take about 4.0g of the test sample (the test sample for determination needs to be crushed to pass through the No. 2 sieve and mixed evenly), accurately weigh, place in a 250mL stoppered conical flask, accurately add 100mL of 50% ethanol, seal, cold soak, shake from time to time within the first 6 hours, and then let stand for 18 hours, quickly filter with a drying filter, accurately measure 20mL of the filtrate, place in an evaporating dish that has been dried to constant weight, evaporate to dryness on a water bath, dry at 105°C for 3 hours, cool in a desiccator for 30 minutes, and quickly and accurately weigh the weight. Unless otherwise specified, the content (%) of alcohol-soluble extracts in the test sample is calculated based on the dry product.

[0074] Example 2 Methodological Investigation

[0075] Linear relationship test

[0076] Based on the chromatographic conditions in Example 1, the liquid chromatograph draws the mixed reference solution respectively, draws the standard curve with the mass concentration as the abscissa (X) and the peak area as the ordinate (Y), and calculates the regression equation.

[0077] In this embodiment, the linear equation, correlation coefficient (r) and linear range are shown in the following Table 1. The results show that the five components have a good linear relationship within their respective ranges.

[0078] Table 1 Results of linear relationship investigation of five components

[0079] Serial number Element Linear equations r Linear range μg / mL 1 Echinacoside y=18075x-0.4439 1 0.87-34.76 2 Cistancheside A y=11791x-0.1981 1 0.45-17.89 3 Verbascum sugar y=17432x-5.5413 0.9999 34.85-1394.12 4 Isovalascoside y=14570x-0.0445 0.9999 0.88-35.15

[0080] Precision test

[0081] Accurately pipette 0.28 mg / mL mixed reference solution, inject and measure continuously 6 times according to the chromatographic conditions in Example 1, and record the peak area.

[0082] In this example, the RSDs of the peak areas of echinacoside, verbascoside, isovalascoside, 2'-acetylverbascoside, and cistancheside A were calculated to be 0.20%, 0.29%, 0.22%, 0.31%, and 0.21%, respectively, indicating that the precision of the instrument is good, the repeatability of the measurement results is high, and the data stability is good.

[0083] Repeatability test

[0084] Accurately weigh 6 portions of the test sample of wine-soaked Cistanche slices, prepare the test solution according to the method in Example 1, continuously inject and measure according to the chromatographic conditions in Example 1, record the peak area, and calculate the RSD value of each component.

[0085] In this example, the average mass fractions of echinacoside, verbascoside, isovalascoside, 2'-acetylverbascoside and cistancheside A were calculated to be 0.03%, 1.65%, 0.02%, 1.26% and 0.01%, respectively, and the RSDs were 1.62%, 0.65%, 3.72%, 0.29% and 3.61%, respectively, indicating that the chromatographic method had good repeatability.

[0086] Stability test

[0087] In this example, a sample solution of 1 portion of salt-raw Cistanche deserticola slices was prepared, and the sample was injected and measured at 0, 2, 4, 6, 8, 12, and 24 h according to the chromatographic conditions in Example 1, the peak areas were recorded, and the RSD values ​​of each component at different times were calculated.

[0088] In this example, the RSDs of the peak areas of echinacoside, verbascoside, isovalascoside, 2'-acetylverbascoside, and cistancheside A were calculated to be 2.62%, 1.04%, 3.90%, 0.71%, and 3.60%, respectively, indicating that the sample solution was stable within 24 hours.

[0089] Sample recovery test

[0090] In this example, 0.5 g of wine-washed Cistanche deserticola powder with a known content of ingredients was weighed and added to each reference solution to prepare 6 test solutions. The samples were injected and measured according to the chromatographic conditions in Example 1, and the average sample recovery rate and RSD value were calculated. The results are shown in Table 2 below.

[0091] The results showed that the recoveries of echinacoside, cistancheside A, verbascoside, isovalascoside and 2'-acetylverbascoside were 100.05%, 108.59%, 100.23%, 97.34% and 97.98%, respectively, and the calculated RSDs were 1.20%, 2.04%, 0.46%, 2.38% and 2.99%, respectively.

[0092] Table 2 Results of sample recovery test

[0093]

[0094] Sample determination

[0095] Weigh 1.00 g of wine-washed Cistanche deserticola slice powder accurately, prepare the test solution according to the method in Example 1, perform the test according to the chromatographic conditions in Example 1, and calculate the content of each index component using the standard curve method. Figure 1-2 ,in, Figure 1 is the chromatogram of the mixed standard solution, Figure 2 The chromatogram of the wine-washed Cistanche decoction piece solution.

[0096] Example 3 Determination of comprehensive evaluation index

[0097] In this embodiment, the correlation of various evaluation indicators in the wine-washed Cistanche deserticola was compared by using the AHP method, the CRITIC method, and the AHP-CRITIC method, the indicator weights were determined, the comprehensive scores were calculated, and a comprehensive scoring model was constructed.

[0098] In this embodiment, the definitions are as follows: the echinacoside content is D X1 , the content of verbascoside is D X2 , the content of iso-verbascoside is D X3 , 2'-acetyl verbascoside content is D X4 , the content of Cistanche deserticola A is D X5, the extract content is D X6 .

[0099] AHP evaluation index

[0100] AHP (Analytic Hierarchy Process) is a multi-criteria decision-making method used to deal with multiple factors and multiple levels in complex problems. Through preliminary experiments, it can be found that the content of verbascoside, 2'-acetylverbascoside and isovalascoside changes significantly after Cistanche deserticola is steamed with wine. At the same time, combined with the requirements and quality markers of wine-processed Cistanche deserticola in the 2020 edition of the "Chinese Pharmacopoeia", three component indicators of Cistanche deserticola A and echinacoside are introduced. According to the increase and decrease of each indicator component before and after the processing of Cistanche deserticola, the content of each indicator component and the content of the extract are quantified as weight indicators. Among them, echinacoside and verbascoside are the main active ingredients of Cistanche deserticola, which are the first level; the content of 2'-acetyl verbascoside increases during the processing process, which is the second level; the extract content is a major indicator for the evaluation of decoction pieces, which is the third level; the content of isovarascoside and cistancheside A is relatively low, and isovarascoside may undergo structural transformation during the processing process, which is an indicator for evaluating Cistanche deserticola decoction pieces, which is the fourth level. According to the increase and decrease of each indicator component before and after the processing of Cistanche deserticola, the content of each indicator component and the extract content are quantified as weight indicators, and the priority order of each indicator is determined as echinacoside = verbascoside > 2'-acetyl verbascoside > extract content > cistancheside A = isovarascoside. A priority judgment matrix for pairwise comparison is constructed, and the consistency ratio factor (CR) = 0.008 < 0.10 is obtained, that is, the priority judgment matrix is ​​established, and the results are shown in Table 3 below.

[0101] The calculation formula of AHP comprehensive score (OD) is OD = D X1 ×0.294+D X2 ×0.294+D X4 ×0.177+D X6 ×0.107+D X5 ×0.064+D X3 ×0.064.

[0102] Table 3 Priority judgment matrix and weight coefficients of pairwise comparison of each evaluation index

[0103]

[0104] CRITIC entropy weight method to calculate weights

[0105] The Critic entropy weight method is an improved method based on the entropy weight method, which is mainly used to deal with the conflict between indicators. In the experiment, there may be mutual conversion between verbascoside, isovalascoside and 2'-acetylverbascoside. In view of the complex mutual conversion phenomenon between chemical components and the need to comprehensively consider the changes of multiple indicators, the Critic entropy weight method can better reflect the importance of each indicator in this complex situation, which is helpful to scientifically analyze the experimental results and make reasonable conclusions. The data in the single factor test of wine washing and salt removal were standardized [indicator component = (measured value-minimum value) / (maximum value-minimum value)], and then the standardized data were imported into SPSSAU for Critic weight analysis. The weight coefficients Wa of echinacoside, verbascoside, 2'-acetylverbascoside, cistancheside A, extract content and isovalascoside were calculated to be 0.178, 0.1003, 0.1261, 0.1888, 0.2676 and 0.1392 respectively.

[0106] Composite weight and comprehensive score determination

[0107] The weight coefficients obtained by the above-mentioned AHP method and CRITIC method are compounded by weight W=Wi*Wa / ∑wi=1Wi*Wa. The compound weight coefficients W of the indicators calculated according to the formula are 0.340, 0.192, 0.145, 0.079, 0.186, and 0.058 respectively.

[0108] The experimental data were standardized and the OD value was calculated, OD = 0.340 × D X1 +0.192×D X2 +0.058×D X3 +0.145×D X4 +0.079×D X5 +0.186×D X6 .

[0109] Comparison of comprehensive evaluation results

[0110] SPSS26.0 software was used to perform correlation analysis on the three comprehensive scores. The results are shown in Table 4 below.

[0111] Table 4 Correlation analysis of weights of wine washing saltiness index

[0112]

[0113] Note: *The correlation is significant at the 0.05 level (two-tailed).

[0114] It can be seen that the correlation coefficient between the AHP method and the AHP-CRITIC method is 0.816 (P<0.05), and the correlation between the two is statistically significant. The correlation coefficient between the CRITIC method and the AHP-CRITIC method is 0.139, and the correlation between the two is not statistically significant. The correlation coefficient between the AHP method and the CRITIC method is -0.407, and the correlation between the two is not statistically significant, that is, the information reflected is not additive. Therefore, the present invention selects the AHP-CRITIC method to determine the indicator weights and calculate the comprehensive score.

[0115] Example 4

[0116] Based on the aforementioned comprehensive scoring model, this embodiment designed a single factor experiment to screen the preparation process of salt-raw Cistanche deserticola wine product.

[0117] This embodiment adopts single-factor experimental design to analyze various processing parameters of wine washing to remove saltiness. In the preliminary experiment, the "water damage" of medicinal materials is taken as the critical point to determine the single-factor investigation range of wine immersion time and wine washing times. The single-factor levels include the type of wine (yellow wine, rice wine, white wine), the ratio of medicinal materials / yellow wine (50g / 25, 50, 75, 100, 150g, i.e. 2:1, 1:1, 1:1.5, 1:2, 1:3), wine immersion time (5, 15, 30, 45, 60, 90min), and the number of wine washings (2, 3, 4, 5, 6 times).

[0118] Wine Types

[0119] Under the conditions of slice / yellow wine ratio of 50g / 75g (1:1.5), wine immersion time of 90min, and wine immersion times of 2 times, the types of wine investigated were yellow wine, rice wine, and white wine, and the content of the extract of the basil cistanche slice washed with wine, the content of the five components, and the OD value were calculated. The results are shown in Table 5 below, and it is found that yellow wine>rice wine>white wine, and yellow wine is selected for subsequent optimization experiments.

[0120] Investigation on the ratio of decoction pieces / yellow wine

[0121] Under the conditions of using yellow wine, wine immersion time of 90min, and wine washing times of 2 times, the ratio of slices / yellow wine was investigated at 50g / 25, 50, 75, 100, and 150g (2:1, 1:1, 1:1.5, 1:2, and 1:3), and the content of the extract of the slices of Cistanche deserticola washed with wine, the content of the five components, and the OD value were calculated. The results are shown in Table 5 below. It can be seen that the amount of slices and yellow wine is 50g / 25g>100>75>50>150g, and the OD value decreases significantly when the amount of yellow wine increases from 25g to 50g, slowly increases from 75g to 100g, and decreases to 150g, showing an overall downward trend. Therefore, the three levels of slices / yellow wine ratios of 50g / 25g, 62.5g, and 100g were selected for subsequent optimization experiments.

[0122] Investigation of wine soaking time

[0123] Under the conditions of using yellow wine as wine type, slices / yellow wine 50g / 75g, and wine washing times twice, the wine immersion time was investigated to be 5, 15, 30, 45, 60, and 90min, respectively, and the content of the extract of the Cistanche deserticola slices washed with wine, the content of the five components, and the OD value were calculated. The results are shown in Table 5 below, and the wine immersion time was 5>15>45>30>60>90min. The wine immersion time ranged from 5 minutes to 90 minutes, and the OD value trend was first reduced, increased at 45 minutes, and then reduced. The three levels of 5, 25, and 45min were selected for subsequent optimization experiments.

[0124] Investigation of the number of wine washing

[0125] Under the conditions of using yellow wine, slices / yellow wine 50g / 75g, and wine immersion time of 90min, the number of wine washings was investigated as 2, 3, 4, 5, and 6 times, and the content of the extract of the basil slices washed with wine, the content of the five components, and the OD value were calculated. The results are shown in Table 5 below, and it is found that 2>3>4>6>5 times, and the number of wine washings decreased significantly from 2 to 5 times, and increased slightly from 6 times. Three levels of 2, 3, and 4 times were selected for subsequent optimization experiments.

[0126] Table 5 Results of single factor test on removing saltiness from wine

[0127]

[0128]

[0129] Example 5

[0130] Based on the aforementioned comprehensive scoring model, this embodiment designed a response surface experiment to screen the preparation process of salt-raw Cistanche deserticola wine product.

[0131] Response Surface Experimental Design

[0132] Based on the results of the above examples, the OD values ​​of the five chemical components and alcohol-soluble extracts were used as response values. According to the Design Expert 11 software, the response surface analysis method with three factors, namely, the ratio of slices / yellow wine (A), wine immersion time (B), and the number of wine washes (C), was used to optimize the optimal processing technology of Cistanche deserticola wine washing to remove saltiness. The response surface was designed based on the results of the single-factor experiment. Fourteen experiments were enhanced by six repetitions to evaluate the pure error. The response surface factor levels, experimental design, and results are shown in Table 6 below.

[0133] Table 6 Response surface factor levels, experimental design and results

[0134]

[0135]

[0136] Model fitting and ANOVA

[0137] This example uses Design Expert 11 software, takes OD value as the response value, performs multiple regression fitting on the three factors A, B, and C, and obtains a binary regression model as shown below:

[0138] Y=8.64-0.1859*A-0.6671*B-0.4894*C-0.5611*AB-0.1812*AC-0.4098*BC+0.7215*A 2 +0.4169*B 2 +0.2959*C 2 ;

[0139] Among them, 8.64, 0.1859, 0.6671, 0.4894, 0.5611, 0.1812, 0.4098, 0.7215, 0.4169, and 0.2959 are the regression coefficients of the intercept term, linear term, interaction term, and quadratic term, respectively, and A, B, and C are independent variables.

[0140] The response surface methodology must evaluate the goodness of fit of the model experimental values ​​in order to achieve better accuracy in the prediction process. The results of the regression model variance analysis are shown in Table 7 below.

[0141] Table 7 Results of variance analysis of regression model

[0142]

[0143]

[0144] It can be seen that the model P = 0.0003 < 0.01, the model is significant, the lack of fit term P = 0.2541 > 0.05, indicating that the lack of fit term is not significant, and the R 2 =0.9168, Radj 2 =0.8420, indicating that the model fits the data well and can be used for prediction and analysis.

[0145] Among the three factors investigated in the processing technology of this example, wine immersion time B (P = 0.0005 < 0.01) and wine washing times C (P = 0.0013 < 0.01) were significant items. Among the interaction items, AB (P = 0.05 < 0.01) and BC (P = 0.0259 < 0.05) were significant items. Among the quadratic items, A 2 (P=0.0002<0.01), B 2 (P=0.016<0.05), C2 (P=0.00649<0.01) is a significant item, indicating that the selected factors and OD values ​​are in a complex linear relationship. According to the F size of each factor, its influence on the comprehensive score is B>C>A.

[0146] 3D surface and contour plot analysis and process prediction

[0147] In this embodiment, the Design Expert 11 software was used to draw a three-dimensional surface map and a contour map, which can clearly reflect the interaction between the wine / cooked slice ratio, the wine immersion time and the number of wine washing times. The three-dimensional response surface curve (AC) and the contour map (AC) are shown in the attached figure. Figure 3-4 shown.

[0148] According to the response surface data analysis, the optimal processing technology for removing saltiness by wine washing is that the ratio of slices / yellow wine is 50g / 99.748g, the wine immersion time is 6.394min, and the number of wine washing is 2.002 times. Under these conditions, the predicted OD value is 11.252.

[0149] Example 6

[0150] This embodiment is verified based on the optimal process test parameters determined in the previous embodiment.

[0151] In this embodiment, combined with actual production, the optimal processing technology of the salt-raw Cistanche deserticola product is adjusted to a slice / yellow wine ratio of 50g / 99g, a wine immersion time of 6min, and a wine washing number of 2 times.

[0152] Three verification tests were conducted on the prepared medicinal pieces according to the above-mentioned preferred process parameters. The experimental results are shown in Table 8 below.

[0153] Table 8 Optimal process conditions test verification results

[0154] Serial number <![CDATA[D X1 %]]> <![CDATA[D X5 %]]> <![CDATA[D X2 %]]> <![CDATA[D X3 %]]> <![CDATA[D X4 %]]> <![CDATA[D X6 %]]> OD 1 0.025 0.012 4.10 0.062 1.24 55.19 11.19 2 0.025 0.011 4.24 0.065 1.28 55.06 11.25 3 0.026 0.011 4.18 0.067 1.24 54.86 11.22 RSD% 2.42 1.68 1.68 4.07 1.77 0.30 0.29

[0155] It can be seen that the measured OD values ​​are 11.19, 11.25, and 11.22, respectively, the calculated average value is 11.22, the RSD is 0.29%, and the OD value is close to the predicted value, indicating that the processing technology of the salt-raw Cistanche deserticola wine product of the present invention is stable.

[0156] Obviously, the above embodiments are merely examples for the purpose of clear explanation, and are not intended to limit the implementation methods. For those skilled in the art, other different forms of changes or modifications can be made based on the above description. It is not necessary and impossible to list all the implementation methods here. The obvious changes or modifications derived therefrom are still within the scope of protection of the invention.

Claims

1. A method for preparing a salt-raw Cistanche deserticola wine product, characterized in that: The method comprises the steps of spraying rice wine on the surface of the raw salt-cooked Cistanche deserticola to soak the product in wine; The mass ratio of the raw salt-cistanche deserticola to rice wine is 2:1-1:2; The wine soaking time is 5-45 minutes, and the wine soaking times are 2-4 times.

2. The method for preparing the salt-raw Cistanche deserticola wine product according to claim 1, characterized in that: The mass ratio of the raw salt-cooked Cistanche deserticola to rice wine is 50g:99g, the wine soaking time is 6 minutes, and the wine soaking times are 2 times.

3. The method for preparing the salt-raw Cistanche deserticola wine product according to claim 1 or 2, characterized in that: The method further comprises the step of drying the raw salt-cistanche deserticola product; Preferably, the temperature of the drying step is 55-60°C.

4. The method for preparing the salt-raw Cistanche deserticola wine product according to any one of claims 1 to 3, characterized in that: The method also includes the steps of constructing a comprehensive scoring model for the salt-raw Cistanche deserticola wine product, and evaluating the quality of the salt-raw Cistanche deserticola wine product based on the comprehensive scoring model.

5. The method for preparing the salt-raw Cistanche deserticola wine product according to claim 4, characterized in that: The comprehensive scoring model of the salt-raw Cistanche deserticola wine product is: OD = 0.340 × D X1 +0.192×D X2 +0.058×D X3 +0.145×D X4 +0.079×D X5 +0.186×D X6 ; Among them, D X1 is the content of echinacoside, D X2 is the verbascoside content, D X3 is the content of isoverbascoside, D X4 is the content of 2'-acetyl verbascoside, D X5 is the content of Cistanche deserticola glycoside A, D X6 It is the extract content of the salt-raw Cistanche deserticola wine product.

6. The method for preparing the salt-raw Cistanche deserticola wine product according to any one of claims 1 to 5, characterized in that: The method further comprises the step of determining the content of the extract of the salt-raw Cistanche deserticola wine product and the effective ingredients of the salt-raw Cistanche deserticola wine product; The active ingredients include echinacoside, verbascoside, isovalascoside, 2'-acetylverbascoside and / or cistancheside A; The method for determining the effective components of the salt-raw Cistanche deserticola wine product comprises high performance liquid chromatography.

7. The method for preparing the salt-raw Cistanche deserticola wine product according to claim 6, characterized in that: The chromatographic conditions of the high performance liquid chromatography method include: using octadecylsilane bonded silica gel as a filler, using acetonitrile as a mobile phase A, using 0.5% acetic acid aqueous solution as a mobile phase B, and performing gradient elution according to the following procedure: 0-6min, A: 10% → 15%, B: 90% → 85%; 6-10min, A: 15% → 18%, B: 85% → 82%; 10-15min, A: 18%, B: 82%; 15-25min, A: 18%→20%, B: 82%→80%; 25-35min, A: 20% → 23%, B: 80% → 77%; 35-37min, A: 23%→10%, B: 77%→90%.

8. The method for preparing the salt-raw Cistanche deserticola wine product according to claim 7, characterized in that: The chromatographic conditions of the high performance liquid chromatography method also include: flow rate 1 min / mL, column temperature 30° C., injection volume 10 μL, and detection wavelength 330 nm.

9. The method for preparing the salt-raw Cistanche deserticola wine product according to any one of claims 6 to 8, characterized in that: The preparation method of the extract of the salt-raw Cistanche deserticola wine product comprises: taking the salt-raw Cistanche deserticola wine product, adding 50v / v% ethanol solution for cold soaking, filtering with a drying filter, and taking the filtrate for evaporation.

10. The method for preparing the salt-raw Cistanche deserticola wine product according to any one of claims 6 to 9, characterized in that: The method further comprises the step of preparing a test solution of the salt-raw Cistanche deserticola wine product; The preparation steps of the test solution include: accurately weighing the salt-raw Cistanche deserticola wine product, adding 50% methanol to soak, adding 50% methanol to make up the weight after ultrasonic treatment, centrifuging and filtering, and collecting the filtrate to obtain the test solution.

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