CN116584649A - Preparation method of low-bitterness ginseng extract and identification method of bitter component in ginseng extract - Google Patents

Preparation method of low-bitterness ginseng extract and identification method of bitter component in ginseng extract Download PDF

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CN116584649A
CN116584649A CN202310270868.2A CN202310270868A CN116584649A CN 116584649 A CN116584649 A CN 116584649A CN 202310270868 A CN202310270868 A CN 202310270868A CN 116584649 A CN116584649 A CN 116584649A
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ginseng extract
bitter
ginseng
raw material
sample
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陈阳
彭婷
李韦琴
马闯
徐剑
王喆
潘凯进
廖子蔚
王鹏
陈志元
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Jing Brand Co ltd
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Abstract

The invention relates to a preparation method of a low-bitterness ginseng extract and an identification method of bitter components in the ginseng extract, wherein the preparation method of the low-bitterness ginseng extract comprises the following steps: (1) Slicing dried Ginseng radix, extracting with ethanol, centrifuging, concentrating, purifying with macroporous resin step by step, and drying to obtain Ginseng radix extract material; (2) Dissolving a proper amount of ginseng extract raw materials with pure water, filtering with a filter membrane, and separating, purifying and drying different functional components corresponding to different fractions in the ginseng extract by using a high-performance liquid chromatograph to obtain 16 high-purity samples; (3) Preparing 16 high-purity samples into solutions by using 50mL pure water respectively, measuring the bitter taste value of each sample by using an electronic tongue, and selecting samples with the bitter taste value more than 0.8; (4) Continuously using high performance liquid chromatograph, collecting the fractions except bitter components in the Ginseng radix extract raw material, and drying to obtain Ginseng radix extract with low bitter degree.

Description

Preparation method of low-bitterness ginseng extract and identification method of bitter component in ginseng extract
Technical Field
The invention relates to the technical field of ginseng extract preparation, in particular to a preparation method of a low-bitterness ginseng extract and an identification method of bitter components in the ginseng extract.
Background
Most foods or drinks with health functions have unpleasant tastes such as bitter tastes. Market research has shown that the acceptance of products by young consumers often depends on the taste of the product, and researchers have been working to explore and identify unpleasant tasting ingredients in the product, and to find corresponding ways to reduce or eliminate such ingredients based on the results of the study.
Bitter taste is one of the most unacceptable taste types for human senses, and has the characteristics of long action time in human body and difficult disappearance compared with other bad tastes (salty taste, sour taste and astringent taste). Ginseng has been confirmed as a conventional plant of medicinal and edible origin to have a bitter taste as its own bad taste, and its source is ginsenoside composed mainly of sugar and carbohydrate.
The ginsenoside has more types and similar basic structures, and can be classified into dammarane type and oleanane type according to different glycosyl structures. Dammarane type is the main type of ginsenoside, and mainly comprises ginsenoside Rb1, rb2, rb3, rc, rd, rg3, rh2, re, rg1, rg2, rf, rh1, etc. The ginsenoside has different components and obvious pharmacological activity, for example, ginsenoside Rg1 can rapidly relieve fatigue, improve learning and memory, delay aging, and has the effects of exciting central nerve and inhibiting platelet aggregation. Ginsenoside Rb2 has effects of promoting DNA and RNA synthesis, inhibiting central nervous system, reducing intracellular calcium, resisting oxidation, scavenging free radicals in vivo, and improving myocardial ischemia reperfusion injury. At present, bitter substances are generally weakened or removed by adopting a macroporous resin method or an activated carbon method, and the principle of the method is that the macroporous resin and the activated carbon are utilized to adsorb bitter substances in the ginseng extract so as to achieve the effect of weakening or removing bitter, but the macroporous resin and the activated carbon can synchronously adsorb more than ten other ginsenoside active ingredients in the ginseng extract in a large amount, so that the pharmacological activity of the prepared ginseng extract is seriously reduced. Therefore, it is important to develop a preparation method of ginseng extract with low bitter taste, which can remove bitter substances in ginseng extract and retain active ingredients in ginseng extract to the greatest extent. Meanwhile, the identification and separation of bitter components in the ginseng extract are of great significance for the definition of the medicinal value.
Disclosure of Invention
The invention aims to solve the problems that the existing ginseng extract prepared in the industry does not remove bitter substances or the active ingredients in ginseng are greatly reduced while the bitter substances are removed, so that the pharmacological activity of the ginseng is seriously reduced, and provides a preparation method of the ginseng extract with low bitter degree and an identification method of bitter ingredients in the ginseng extract.
The preparation method of the ginseng extract with low bitterness comprises the following steps:
(1) Preparing ginseng extract raw materials: firstly, slicing the dried ginseng, extracting with ethanol, collecting an extracting solution, centrifuging, concentrating, purifying step by step with macroporous resin, and drying to obtain a ginseng extract raw material;
(2) Separating, purifying and drying main functional components of the ginseng extract raw material: dissolving the ginseng extract raw material prepared in the step (1) in 1 g by using pure water, filtering the ginseng extract raw material by using a filter membrane, collecting filtrate, separating, purifying and drying different main functional components corresponding to different fractions in the ginseng extract raw material by using a high-efficiency preparation liquid chromatograph to obtain 16 high-purity samples with the number of 1-16 respectively;
(3) Electronic tongue bitterness determination: preparing the 16 high-purity samples prepared in the step (2) into solutions by using 50mL pure water respectively, measuring the bitter taste value of each sample by using an electronic tongue, and selecting samples with the bitter taste value more than 0.8;
(4) Preparation of ginseng extract with low bitterness: under the condition of determining the bitter component sample in the ginseng extract raw material, continuously using a high performance liquid chromatograph, respectively collecting and drying the fraction of the bitter component and the fraction except for the bitter component in the ginseng extract raw material, wherein the extract obtained from the fraction except for the bitter component is the low-bitter-degree ginseng extract, and the extract corresponding to the fraction of the bitter component is singly collected.
Preferably, in the step (1), the concentration of the ethanol solution is 70% -85%, and the mass-volume ratio of the ginseng to the ethanol solution is 1:10-20, wherein the extraction times are 1-3 times, the extraction time is 1-4 h each time, the extraction temperature is 50-65 ℃, the centrifugal speed is 5000-7000 r/min, the centrifugal time is 10-15 min, the centrifugal supernatant is concentrated to 1/20-1/10 of the original volume, the D101 type macroporous resin collecting part is eluent, the D941 type weak alkaline anion exchange resin collecting part is permeate, the used resins are D101 type macroporous resin and D941 type weak alkaline anion exchange resin respectively, the eluting solvent is 50-65% ethanol solution, the eluting solvent consumption is 3-6 BV, the eluent flow rate is 0.5-1.0 BV/h, the permeate flow rate is 0.8-1.2BV/h, the drying mode is low-temperature vacuum drying or vacuum freeze drying, and the total saponin content of the obtained ginseng extract raw material is more than 60%.
Preferably, in the step (2), the final dissolution concentration of the ginseng extract raw material is 5-10 mg/mL, the pore diameter of the filter membrane is 0.22-0.5 μm, the main functional components in the ginseng extract raw material are separated and purified and then dried in a vacuum freeze-drying or low-temperature vacuum drying mode, and the chromatographic conditions of the high-performance preparation liquid chromatograph are as follows: chromatographic column: eclipse XDB-C18 chromatographic column or Daisogel C18 chromatographic column with detection wavelength of 200-300 nm, and mobile phase elution gradient of high performance liquid chromatograph as follows:
preferably, in the step (3), the number of measurements per sample using the electronic tongue is 3 to 5.
In the step (4), the distribution time period of the fraction of bitter component in the ginseng extract raw material is 44.000 min-45.700 min and 74.300min-76.350 min; the low bitterness ginseng extract is collected and dried to obtain fractions except for the time period of 44.000 min-45.700 min and 74.300min-76.350 min.
The identification method of bitter components in ginseng extract comprises the following steps:
(1) Preparing ginseng extract raw materials: firstly, slicing the dried ginseng, extracting with ethanol, collecting an extracting solution, centrifuging, concentrating, purifying step by step with macroporous resin, and drying to obtain a ginseng extract raw material;
(2) Separating, purifying and drying main functional components of the ginseng extract raw material: dissolving the ginseng extract raw material prepared in the step (1) in 1 g by using pure water, filtering the ginseng extract raw material by using a filter membrane, collecting filtrate, separating, purifying and drying different main functional components corresponding to different fractions in the ginseng extract raw material by using a high-efficiency preparation liquid chromatograph to obtain 16 high-purity samples with the number of 1-16 respectively;
(3) Electronic tongue bitterness determination: preparing the 16 high-purity samples prepared in the step (2) into solutions by using 50mL pure water respectively, measuring the bitter taste value of each sample by using an electronic tongue, and selecting samples with the bitter taste value more than 0.8;
(4) Liquid chromatography-mass spectrometry identification of bitter components: filtering the sample solution with bitter value more than 0.8 with a filter membrane, and measuring by liquid chromatography-mass spectrometry to estimate the components of the sample;
(5) And (3) determining the matching degree of the bitter component reference substance: and (3) according to the ingredients estimated in the step (4), comparing the peak-out time of the sample solution with the bitterness value of more than 0.8 by using a standard substance, and finally determining the bitterness ingredients in the ginseng extract raw material.
Preferably, in step (4), the liquid chromatography-mass spectrometry detection conditions are: chromatographic column: waters ACQUITY UPLC HSS T3C 18 column, flow rate of 0.4-0.6 mL/min, column temperature of 30-40 ℃, and sample injection amount of: control 0.08-0.1. Mu.L, sample solution 0.2-0.4. Mu.L, mobile phase: a is 0.1% formic acid water solution, B is 0.1% formic acid acetonitrile solution, and the mobile phase elution gradient is:
in the step (4), the relative error of the peak time of the standard substance and the sample with the bitter value more than 0.8 is not more than 3 percent.
The technological principle of the method of the invention is as follows: extracting a ginseng extract raw material by a common extraction method, then taking a sample, adopting high-efficiency preparation liquid chromatography, separating, purifying and drying main functional components in the ginseng extract raw material to obtain 16 high-purity samples with the numbers of 1-16 respectively, preparing solutions by using 50mL of pure water respectively for the 16 high-purity samples (the contents of different samples in the ginseng extract raw material are different, the same amount of pure water is used for dissolving, the prepared solution concentration can be ensured to correspond to the contents of different samples in the ginseng extract raw material, the measured bitter taste value only has a reference value), and measuring the bitter taste value of each sample by an electronic tongue to select the sample with the bitter taste value more than 0.8; the fraction time period corresponding to the sample with the bitterness value greater than 0.8 is the fraction period of the ginseng extract with high bitterness, and is required to be collected independently; collecting the fraction except for the fraction time period corresponding to the sample with bitterness value greater than 0.8, and drying to obtain Ginseng radix extract with low bitterness. Meanwhile, the invention also adopts liquid chromatography-mass spectrometry to identify bitter components in the ginseng extract raw material, and uses a standard substance to compare the peak time of a sample with the bitter value more than 0.8, so as to finally determine that the bitter components in the ginseng extract raw material are ginsenoside Rb1 and ginsenoside Rg1, and the bitter components are collected and dried independently, thus providing a beneficial basis for the medicinal value of the bitter components in the ginseng extract.
The beneficial effects of the invention are as follows:
1. the preparation process is feasible as a whole, strong in operability and simple and feasible: the invention adopts high performance liquid chromatography to prepare the ginseng extract with low bitterness, the preparation process has strong repeatability, and the preparation process is simple and easy to implement.
2. The research of the invention shows that not all ginsenoside component types have strong bitter taste, and the component types with high bitter taste in ginseng are defined, so that the invention has important significance for removing or reducing the bitter taste of ginseng-containing products and ginseng extracts.
3. The identification degree of bitter components in the ginseng extract is accurate, and the result is reliable: according to the invention, the high-efficiency preparation liquid chromatograph is utilized to directly separate and purify each bitter component in the ginseng extract, the purity of the obtained sample is high, and the liquid chromatography-mass spectrometry and the common liquid chromatography are utilized to carry out component identification on the bitter components, so that the specific types of the removed bitter components are completely understood by production staff, and data support is provided for the subsequent pharmacological application of the low-bitter ginseng extract and the high-bitter ginseng extract components (ginsenoside Rb1 and ginsenoside Rg 1).
4. The obtained low-bitter ginseng extract has low bitter value, and increases application range of low-bitter ginseng extract.
5. Compared with the conventional macroporous resin debitterizing method or the activated carbon debitterizing method, the method disclosed by the invention not only can remove the bitter taste in the ginseng extract, but also can maximally retain the functional components in the ginseng extract.
Drawings
FIG. 1 is a liquid chromatogram of the ginseng extract raw material of example 1 of the present invention when it is separated and purified by high performance preparative liquid chromatography;
FIG. 2 is a comparison of the off-peak time liquid chromatograms of a comparison standard and sample No. 1 using a common liquid chromatograph in example 5 of the present invention;
FIG. 3 is a comparison of the peak time liquid chromatograms of the standard and sample No. 6 compared in example 5 of the present invention using a common liquid chromatograph.
Detailed Description
In order to better explain the technical solution of the present invention, the following description of the technical solution of the present invention is given by way of example only and not by way of limitation in any way, in conjunction with specific examples. All changes and equivalents that do not depart from the gist of the invention are intended to be within the scope of the invention.
The preparation method of the ginseng extract with low bitterness comprises the following steps:
(1) Preparing ginseng extract raw materials: firstly, slicing the dried ginseng, and extracting for 1-3 times by using 70-85% ethanol solution with the mass-volume ratio of 1:10-20, extracting at 50-65deg.C for 1-4 h, mixing the extractive solutions, centrifuging at 5000-7000 r/min for 10-15 min to obtain supernatant, concentrating the supernatant to 1/20-1/10 of original volume, loading on D101 macroporous resin column, eluting with 3-6 BV 50-65% ethanol solution at a flow rate of 0.5-1.0 BV/h, collecting eluate on D941 type weakly basic anion exchange resin column, collecting the permeate at a flow rate of 0.8-1.2BV/h, collecting the permeate as purified centrifugate, and vacuum freeze drying or low-temperature vacuum drying to obtain Ginseng radix extract material with total saponin content of > 60%;
(2) Separating, purifying and drying main functional components of the ginseng extract raw material: taking the ginseng extract raw material prepared in the step (1) of 1 g, dissolving the ginseng extract raw material into a ginseng extract solution with a final concentration of 5-10 mg/mL by using pure water, filtering the ginseng extract solution by using a 0.22-0.5 mu m filter membrane, collecting filtrate, separating, purifying and drying different main functional components corresponding to different fractions in the ginseng extract raw material by using a high-performance liquid chromatograph to obtain 16 high-purity samples, wherein the samples are respectively numbered 1-16, and the conditions of the high-performance liquid chromatograph are as follows: chromatographic column: daisogelC18 column, detection wavelength 203 nm, mobile phase elution gradient:
(3) Electronic tongue bitterness determination: preparing the 16 high-purity samples prepared in the step (2) into solutions by using 50mL pure water respectively, measuring the bitter taste value of each sample by using an electronic tongue, and selecting samples with the bitter taste value more than 0.8;
(4) Preparation of ginseng extract with low bitterness: under the condition of determining a bitter component sample in the ginseng extract raw material, continuously using a high performance liquid chromatograph, respectively collecting and drying fractions of bitter components and fractions except for the bitter components in the ginseng extract raw material, wherein extracts obtained from the fractions except for the bitter components are low-bitter-degree ginseng extracts, and extracts corresponding to the fractions of the bitter components are independently collected; the distribution time period of the fraction corresponding to bitter component of Ginseng radix extract raw material is 44.000 min-45.700 min and 74.300min-76.350 min; the low bitterness ginseng extract is collected and dried to obtain fractions except for the time period of 44.000 min-45.700 min and 74.300min-76.350 min.
The identification method of bitter components in the ginseng extract is carried out continuously on the basis of the preparation method of the ginseng extract with low bitter degree, and comprises the following steps of:
(1) Liquid chromatography-mass spectrometry identification of bitter components: filtering the sample solution with bitter value more than 0.8 with a filter membrane, and measuring by liquid chromatography-mass spectrometry to estimate the components of the sample; the detection conditions of the liquid chromatography-mass spectrometry are as follows: chromatographic column: waters ACQUITY UPLC HSS T3C 18 column, flow rate of 0.4-0.6 mL/min, column temperature of 30-40 ℃, and sample injection amount of: control 0.08-0.1. Mu.L, sample solution 0.2-0.4. Mu.L, mobile phase: a is 0.1% formic acid water solution, B is 0.1% formic acid acetonitrile solution, and the mobile phase elution gradient is:
estimating specific substances represented by bitter components according to the results of liquid chromatography-mass spectrometry data;
(2) And (3) determining the matching degree of the bitter component reference substance: and finally determining the bitter component in the ginseng extract by comparing the standard substance with the peak time of a sample solution with the bitter value more than 0.8, wherein the relative error of the peak time of the standard substance and the sample with the bitter value more than 0.8 is not more than 3 percent.
Example 1
A method for preparing Ginseng radix extract with low bitterness comprises the following steps:
(1) Preparing ginseng extract raw materials: firstly, slicing dried ginseng 0.5 and kg, extracting for 2 times by using an ethanol solution with the mass fraction of 80%, wherein the mass-volume ratio of the ginseng to the ethanol solution is 1:10, extracting at 65 ℃ each time for 2 h, combining the extracting solutions, centrifuging for 15 min under the centrifugal condition of 7000 r/min to obtain a centrifugate, concentrating the centrifugate to 1L, then loading on a D101 macroporous resin column, eluting with a 50% ethanol solution of 3L, loading on a D941 type weak alkaline anion exchange resin column at the eluent flow rate of 0.5L/h, allowing the permeate flow rate of 0.8L/h, collecting the permeate to obtain a purified solution, and performing vacuum freeze drying on the obtained purified solution to obtain 10.2g of ginseng extract with the total saponin content of 75%;
(2) Separating, purifying and drying main functional components of the ginseng extract raw material: taking the ginseng extract raw material prepared in the step (1) of 1 g, dissolving the ginseng extract raw material into a ginseng extract solution with a final concentration of 5 mg/mL by using pure water, filtering the ginseng extract solution by using a 0.22 mu m filter membrane, collecting filtrate, separating, purifying and drying different main functional components corresponding to different fractions in the ginseng extract raw material by using a high-efficiency preparation liquid chromatograph to obtain 16 high-purity samples, and respectively numbering the samples to be 1-16 according to the peak outlet sequence (see the attached figure 1, wherein the high-efficiency preparation liquid chromatograph is used for separating and purifying the ginseng extract raw material prepared in the embodiment 1), and the conditions of the high-efficiency preparation liquid chromatograph are as follows: chromatographic column: daisogelC18 column, detection wavelength 203 nm, mobile phase elution gradient:
(3) Electronic tongue bitterness determination: preparing the 16 high-purity samples prepared in the step (2) into solutions by using 50mL pure water respectively, measuring the bitter taste value of each sample by using an electronic tongue, measuring the number of times of each sample by using the electronic tongue for 3 times, taking an average value as a measurement result (see table 1 below), and selecting samples with the bitter taste value more than 0.8;
table 1 shows a Table (average) of bitter taste values of 16 functional components of the ginseng extract
As can be seen from table 1, the bitter values of sample No. 1 and sample No. 6 are relatively high, both are much greater than 0.8, and are much greater than the bitter values of the other components, indicating that components No. 1 and 6 are the main bitter substances in the ginseng extract;
(4) Preparation of ginseng extract with low bitterness: under the condition of determining a bitter component sample in the ginseng extract, continuously using a high performance liquid chromatograph to respectively collect and dry fractions of bitter components and fractions except for the bitter components in the ginseng extract raw material, wherein the extracts obtained from the fractions except for the bitter components are low-bitter-degree ginseng extracts, and the extracts corresponding to the fractions of the bitter components are independently collected as high-bitter-degree ginseng extract components; the distribution time period of fraction corresponding to bitter component in Ginseng radix extract raw material is 44.000 min-45.700 min (sample No. 1) and 74.300min-76.350 min (sample No. 6); the low bitterness ginseng extract is collected and dried to obtain fractions except for the time period of 44.000 min-45.700 min and 74.300min-76.350 min.
Taking the raw materials of the ginseng extract prepared in the step (1) of example 1 and the low-bitter ginseng extract prepared in the step (4), respectively preparing solutions with the content of the ginseng extract of 5 mg/mL by pure water, respectively tasting the bitter taste values of two samples by an electronic tongue 3 times, taking the average value of the three times, and measuring the average value as shown in the following table 2, wherein the bitter taste value of the low-bitter ginseng extract prepared by the method of the invention is remarkably reduced compared with that of the ginseng extract prepared by the conventional extraction.
TABLE 2 example 1 results of bitterness test of Low bitterness Ginseng radix extract and Ginseng radix extract raw Material
Example 2
A method for preparing Ginseng radix extract with low bitterness comprises the following steps:
(1) Preparing ginseng extract raw materials: firstly, slicing 0.5kg of dried ginseng, extracting 3 times by using 70% ethanol solution with the mass fraction of 1:15, extracting at 50 ℃ each time, extracting 4 h, combining the extracting solutions, centrifuging at 6000 r/min for 13 min to obtain a centrifugate, concentrating the centrifugate to 1L, then loading on a D101 macroporous resin column, eluting with 3L 55% ethanol solution, collecting the eluate, loading on a D941 weak-alkaline anion exchange resin column at the flow rate of 0.6L/h, enabling the flow rate of the permeate to be 0.85L/h, collecting the permeate to obtain a purified solution, and performing vacuum freeze drying on the obtained purified solution to obtain 10.8 g of the ginseng extract with the total saponin content of 77%;
(2) Separating, purifying and drying main functional components of the ginseng extract raw material: taking the ginseng extract raw material prepared in the step (1) of 1 g, dissolving the ginseng extract raw material into a ginseng extract solution with a final concentration of 10 mg/mL by using pure water, filtering the ginseng extract solution by using a 0.5 mu m filter membrane, collecting filtrate, separating, purifying and drying different main functional components corresponding to different fractions in the ginseng extract raw material by using a high-efficiency preparation liquid chromatograph to obtain 16 high-purity samples, and respectively numbering the samples to be 1-16 according to a peak outlet sequence, wherein the high-efficiency preparation liquid chromatograph conditions are as follows: chromatographic column: daisogelC18 column, detection wavelength 203 nm, mobile phase elution gradient as in example 1;
(3) Electronic tongue bitterness determination: preparing the 16 high-purity samples prepared in the step (2) into solutions by using 50mL pure water respectively, measuring the bitter taste value of each sample by using an electronic tongue, measuring the number of times of each sample by using the electronic tongue for 4 times, taking an average value as a measurement result, and selecting samples with the bitter taste value more than 0.8, wherein the samples with higher bitter taste values are samples No. 1 and No. 6;
(4) Preparation of ginseng extract with low bitterness: under the condition of determining a bitter component sample in the ginseng extract, continuously using a high performance liquid chromatograph to respectively collect and dry fractions of bitter components and fractions except for the bitter components in the ginseng extract raw material, wherein the extracts obtained from the fractions except for the bitter components are low-bitter-degree ginseng extracts, and the extracts corresponding to the fractions of the bitter components are independently collected as high-bitter-degree ginseng extract components; the distribution time period of fraction corresponding to bitter component in Ginseng radix extract raw material is 44.000 min-45.700 min (sample No. 1) and 74.300min-76.350 min (sample No. 6); the low bitterness ginseng extract is collected and dried to obtain fractions except for the time period of 44.000 min-45.700 min and 74.300min-76.350 min.
Taking the raw materials of the ginseng extract prepared in the step (1) of example 2 and the low-bitter ginseng extract prepared in the step (4), preparing solutions of the ginseng extract with the content of 5 mg/mL respectively by pure water, then tasting the bitter taste values of the two samples by an electronic tongue 5 times respectively, taking the average value of 5 times, and measuring the average value as shown in the following table 3, wherein the bitter taste value of the low-bitter ginseng extract prepared by the method of the invention is remarkably reduced compared with that of the ginseng extract prepared by the conventional extraction.
TABLE 3 example 2 results of bitterness test of Low bitterness Ginseng radix extract and Ginseng radix extract raw Material
Example 3
A method for preparing Ginseng radix extract with low bitterness comprises the following steps:
(1) Preparing ginseng extract raw materials: firstly, slicing dried ginseng 0.5 and kg, extracting for 1 time by using an ethanol solution with the mass fraction of 85%, wherein the mass-volume ratio of the ginseng to the ethanol solution is 1:20, extracting at 55deg.C for 3 h each time, mixing the extractive solutions, centrifuging at 5000 r/min for 10min to obtain centrifugate, concentrating the centrifugate to 1.3L, loading onto D101 macroporous resin column, eluting with 3L ethanol solution of 65%, collecting eluate, loading onto D941 weak alkaline anion exchange resin column at flow rate of 0.7L/h, collecting the permeate at flow rate of 0.9L/h to obtain purified solution, and vacuum freeze drying to obtain Ginseng radix extract 9.8 g with total saponin content of 80%;
(2) Separating, purifying and drying main functional components of the ginseng extract raw material: taking the ginseng extract raw material prepared in the step (1) of 1 g, dissolving the ginseng extract raw material into a ginseng extract solution with a final concentration of 8 mg/mL by using pure water, filtering the ginseng extract solution by using a 0.3 mu m filter membrane, collecting filtrate, separating, purifying and drying different main functional components corresponding to different fractions in the ginseng extract raw material by using a high-efficiency preparation liquid chromatograph to obtain 16 high-purity samples, and respectively numbering the samples into numbers 1-16 according to a peak outlet sequence, wherein the high-efficiency preparation liquid chromatograph conditions are as follows: chromatographic column: daisogelC18 column, detection wavelength 203 nm, mobile phase elution gradient as in example 1;
(3) Electronic tongue bitterness determination: preparing the 16 high-purity samples prepared in the step (2) into solutions by using 50mL pure water respectively, measuring the bitter taste value of each sample by using an electronic tongue, measuring the number of times of each sample by using the electronic tongue for 5 times, taking an average value as a measurement result, and selecting samples with the bitter taste value more than 0.8, wherein the samples with higher bitter taste values are samples No. 1 and No. 6;
(4) Preparation of ginseng extract with low bitterness: under the condition of determining a bitter component sample in the ginseng extract, continuously using a high performance liquid chromatograph to respectively collect and dry fractions of bitter components and fractions except for the bitter components in the ginseng extract raw material, wherein the extracts obtained from the fractions except for the bitter components are low-bitter-degree ginseng extracts, and the extracts corresponding to the fractions of the bitter components are independently collected as high-bitter-degree ginseng extract components; the distribution time period of fraction corresponding to bitter component in Ginseng radix extract raw material is 44.000 min-45.700 min (sample No. 1) and 74.300min-76.350 min (sample No. 6); the low bitterness ginseng extract is collected and dried to obtain fractions except for the time period of 44.000 min-45.700 min and 74.300min-76.350 min.
Taking the raw materials of the ginseng extract prepared in the step (1) of example 3 and the low-bitter ginseng extract prepared in the step (4), preparing solutions of the ginseng extract with the content of 5 mg/mL respectively by pure water, then tasting the bitter taste values of the two samples by an electronic tongue for 4 times respectively, taking the average value of the 4 times, and determining the results as shown in the following table 4, wherein the bitter taste values of the low-bitter ginseng extract prepared by the method of the invention are remarkably reduced compared with those of the ginseng extract prepared by the conventional extraction.
TABLE 4 example 3 results of bitterness test of Low bitterness Ginseng radix extract and Ginseng radix extract raw Material
Example 4
A method for preparing Ginseng radix extract with low bitterness comprises the following steps:
(1) Preparing ginseng extract raw materials: firstly, slicing dried ginseng 0.5-kg, extracting 3 times by using an ethanol solution with the mass fraction of 75%, wherein the mass-volume ratio of the ginseng to the ethanol solution is 1:18, extracting at 60 ℃ each time for 1 h, combining the extracting solutions, centrifuging for 12min under the centrifugal condition of 6500 r/min to obtain a centrifugate, concentrating the centrifugate to 1.2L, then loading on a D101 macroporous resin column, eluting with a 60% ethanol solution of 3L, loading on a D941 type weak alkaline anion exchange resin column at the eluent flow rate of 0.6L/h, collecting the eluent to obtain a permeate at the permeate flow rate of 0.88L/h, collecting the permeate to obtain a purified solution, and performing vacuum freeze drying on the obtained purified solution to obtain a ginseng extract 10.3 g with the total saponin content of 78%;
(2) Separating, purifying and drying main functional components of the ginseng extract raw material: taking the ginseng extract raw material prepared in the step (1) of 1 g, dissolving the ginseng extract raw material into a ginseng extract solution with a final concentration of 10 mg/mL by using pure water, filtering the ginseng extract solution by using a 0.22 mu m filter membrane, collecting filtrate, separating, purifying and drying different main functional components corresponding to different fractions in the ginseng extract raw material by using a high-efficiency preparation liquid chromatograph to obtain 16 high-purity samples, and respectively numbering the samples to be 1-16 according to a peak outlet sequence, wherein the high-efficiency preparation liquid chromatograph conditions are as follows: chromatographic column: daisogelC18 column, detection wavelength 203 nm, mobile phase elution gradient as in example 1;
(3) Electronic tongue bitterness determination: preparing the 16 high-purity samples prepared in the step (2) into solutions by using 50mL pure water respectively, measuring the bitter taste value of each sample by using an electronic tongue, measuring the number of times of each sample by using the electronic tongue for 3 times, taking an average value as a measurement result, and selecting samples with the bitter taste value more than 0.8, wherein the samples with higher bitter taste values are samples No. 1 and No. 6;
(4) Preparation of ginseng extract with low bitterness: under the condition of determining a bitter component sample in the ginseng extract, continuously using a high performance liquid chromatograph to respectively collect and dry fractions of bitter components and fractions except for the bitter components in the ginseng extract raw material, wherein the extracts obtained from the fractions except for the bitter components are low-bitter-degree ginseng extracts, and the extracts corresponding to the fractions of the bitter components are independently collected as high-bitter-degree ginseng extract components; the distribution time period of fraction corresponding to bitter component in Ginseng radix extract raw material is 44.000 min-45.700 min (sample No. 1) and 74.300min-76.350 min (sample No. 6); the low bitterness ginseng extract is collected and dried to obtain fractions except for the time period of 44.000 min-45.700 min and 74.300min-76.350 min.
Taking the ginseng extract raw material obtained in the step (1) of example 4 and the low-bitterness ginseng extract obtained in the step (4), preparing solutions of 5 mg/mL of ginseng extract with pure water respectively, tasting the bitter taste values of the two samples with electronic tongues respectively for 3 times, taking the average value of 3 times, and measuring the results as shown in the following table 4: the low-bitterness ginseng extract prepared by the method of the invention has significantly reduced bitterness value compared with the ginseng extract prepared by conventional extraction.
TABLE 5 example 5 results of bitterness test of Low bitterness Ginseng radix extract and Ginseng radix extract raw Material
As can be seen from the above examples 1-4, the low bitterness ginseng extract prepared by the method of the present invention has a bitterness value reduced by more than 96% as compared with the ginseng extract prepared by conventional extraction, indicating that the method of the present invention is practical in reducing the bitterness of ginseng extract.
Example 5
A method for identifying bitter component in Ginseng radix extract by using sample solution 1 and sample solution 6 selected in step (3) of example 1 comprises the following steps:
(1) Liquid chromatography-mass spectrometry identification of bitter components: filtering sample solutions No. 1 and No. 6 with bitter taste value greater than 0.8 with filter membrane, respectively, and measuring by liquid chromatography-mass spectrometry to estimate the components of sample No. 1 and sample No. 6; the detection conditions of the liquid chromatography-mass spectrometry are as follows: chromatographic column: waters ACQUITYUPLC HSS T3C 18 column, flow rate of 0.4-0.6 mL/min, column temperature of 30-40 ℃, and sample injection amount of: control 0.08-0.1. Mu.L, sample solution 0.2-0.4. Mu.L, mobile phase: a is 0.1% formic acid water solution, B is 0.1% formic acid acetonitrile solution, and the mobile phase elution gradient is:
the results of the liquid chromatography-mass spectrometry experiments are shown in table 6 below:
TABLE 6 Mass Spectrometry parameters for sample No. 1 and sample No. 6 with higher bitterness value in example 1
Comparing the mass spectrum parameters of sample No. 1 and sample No. 6 with the mass spectrum parameter data in the literature, it is presumed that sample No. 1 may be ginsenoside Rg1, and sample No. 6 may be ginsenoside Rb1.
(2) And (3) determining the matching degree of the bitter component reference substance: and (3) respectively comparing peak-out time of the standard substance with that of the No. 1 sample and that of the No. 6 sample solution by using a common liquid chromatograph, wherein test results are shown in the accompanying drawings 2 and 3.
As can be seen from fig. 2 and fig. 3, the peak time of the sample No. 1 is substantially the same as that of the ginsenoside Rg1 standard, the peak time of the sample No. 6 is substantially the same as that of the ginsenoside Rb1 standard, and the sample No. 1 is ginsenoside Rg1 and the sample No. 6 is ginsenoside Rb1, which are proved by the connection of mass spectrum parameter data. By adopting the method of example 5, the sample No. 1 and the sample No. 6 in examples 2-4 are identified by liquid chromatography-mass spectrometry, and the peak time of the standard substance and the sample No. 1 and the peak time of the sample No. 6 are compared by using a common liquid chromatograph, and the results show that the sample No. 1 contains ginsenoside Rg1 and the sample No. 6 contains ginsenoside Rb1. The bitter components in the ginseng extract are proved to be ginsenoside Rb1 and ginsenoside Rg1.
The above examples are merely illustrative of preferred embodiments of the present invention and do not include all embodiments of the invention. Various modifications and alterations may be made by those skilled in the art without departing from the spirit and scope of the invention, which is to be considered as falling within the scope of the appended claims.

Claims (10)

1. A preparation method of a ginseng extract with low bitterness is characterized by comprising the following steps:
(1) Preparing ginseng extract raw materials: firstly, slicing the dried ginseng, extracting with ethanol, collecting an extracting solution, centrifuging to obtain a supernatant, concentrating, purifying step by step with macroporous resin, and drying to obtain a ginseng extract raw material;
(2) Separating, purifying and drying main functional components of the ginseng extract raw material: dissolving the ginseng extract raw material prepared in the step (1) in 1 g by using pure water, filtering the ginseng extract raw material by using a filter membrane, collecting filtrate, separating, purifying and drying different main functional components corresponding to different fractions in the ginseng extract raw material by using a high-efficiency preparation liquid chromatograph to obtain 16 high-purity samples with the number of 1-16 respectively;
(3) Electronic tongue bitterness determination: preparing the 16 high-purity samples prepared in the step (2) into solutions by using 50mL pure water respectively, measuring the bitter taste value of each sample by using an electronic tongue, and selecting samples with the bitter taste value more than 0.8;
(4) Preparation of ginseng extract with low bitterness: under the condition of determining the bitter component sample in the ginseng extract raw material, continuously using a high performance liquid chromatograph, respectively collecting and drying the fraction of the bitter component and the fraction except for the bitter component in the ginseng extract raw material, wherein the extract obtained from the fraction except for the bitter component is the low-bitter-degree ginseng extract, and the extract corresponding to the fraction of the bitter component is singly collected.
2. The method for preparing a ginseng extract with low bitterness according to claim 1, wherein: in the step (1), the concentration of the ethanol solution is 70-85%, and the mass volume ratio of the ginseng to the ethanol solution is 1:10-20, wherein the extraction times are 1-3 times, the extraction time is 1-4 h each time, the extraction temperature is 50-65 ℃, the centrifugal speed is 5000-7000 r/min, the centrifugal time is 10-15 min, the centrifugal supernatant is concentrated to 1/20-1/10 of the original volume, the D101 macroporous resin collecting part is eluent, the D941 weak alkaline anion exchange resin collecting part is permeate, the used resins are D101 macroporous resin and D941 weak alkaline anion exchange resin respectively, the eluting solvent is 50-65% ethanol solution, the eluting solvent dosage is 3-6 BV, the eluent flow rate is 0.5-1.0 BV/h, the permeate flow rate is 0.8-1.2BV/h, and the drying mode is low-temperature vacuum drying or vacuum freeze drying.
3. The method for preparing a ginseng extract with low bitterness according to claim 1, wherein: in the step (1), the total saponin content in the obtained ginseng extract raw material is more than 60 percent.
4. The method for preparing a ginseng extract with low bitterness according to claim 1, wherein: in the step (2), the dissolution final concentration of the ginseng extract raw material is 5-10 mg/mL, the pore diameter of a filter membrane is 0.22-0.5 mu m, the main functional components in the ginseng extract raw material are subjected to vacuum freeze drying or low-temperature vacuum drying after separation and purification, and the chromatographic conditions of a high-performance liquid chromatograph are as follows: chromatographic column: eclipse XDB-C18 chromatographic column or Daisogel C18 chromatographic column, detection wavelength is 200-300 nm.
5. The method for preparing a ginseng extract with low bitterness according to claim 1, wherein: in the step (2), the mobile phase elution gradient of the high performance liquid chromatograph is as follows:
。
6. the method for preparing a ginseng extract with low bitterness according to claim 1, wherein: in the step (3), the number of times of measurement of each sample by using the electronic tongue is 3-5 times.
7. The method for preparing a ginseng extract with low bitterness according to claim 1, wherein: the distribution time period of the bitter component of the Ginseng radix extract material is 44.000 min-45.700 min and 74.300min-76.350 min; the low bitterness ginseng extract is collected and dried to obtain fractions except for the time period of 44.000 min-45.700 min and 74.300min-76.350 min.
8. A method for identifying bitter components in ginseng extract, which is characterized by comprising the following steps:
(1) Preparing ginseng extract raw materials: firstly, slicing the dried ginseng, extracting with ethanol, collecting an extracting solution, centrifuging, concentrating, purifying step by step with macroporous resin, and drying to obtain a ginseng extract raw material;
(2) Separating, purifying and drying main functional components of the ginseng extract raw material: dissolving the ginseng extract raw material prepared in the step (1) in 1 g by using pure water, filtering the ginseng extract raw material by using a filter membrane, collecting filtrate, separating, purifying and drying main functional components in the ginseng extract raw material by using a high performance liquid chromatograph to obtain 16 high-purity samples with the number of 1-16 respectively;
(3) Electronic tongue bitterness determination: preparing the 16 high-purity samples prepared in the step (2) into solutions by using 50mL pure water respectively, measuring the bitter taste value of each sample by using an electronic tongue, and selecting samples with the bitter taste value more than 0.8;
(4) Liquid chromatography-mass spectrometry identification of bitter components: filtering the sample solution with bitter value more than 0.8 with a filter membrane, and measuring by liquid chromatography-mass spectrometry to estimate the components of the sample;
(5) And (3) determining the matching degree of the bitter component reference substance: and (3) according to the ingredients estimated in the step (4), comparing the peak-out time of the sample solution with the bitterness value of more than 0.8 by using a standard substance, and finally determining the bitterness ingredients in the ginseng extract raw material.
9. The method for identifying bitter components in a ginseng extract according to claim 8, wherein: in the step (4), the detection conditions of the liquid chromatography-mass spectrometry are as follows: chromatographic column: waters ACQUITY UPLC HSS T3C 18 column, flow rate of 0.4-0.6 mL/min, column temperature of 30-40 ℃, and sample injection amount of: control 0.08-0.1. Mu.L, sample solution 0.2-0.4. Mu.L, mobile phase: a is 0.1% formic acid water solution, B is 0.1% formic acid acetonitrile solution, and the mobile phase elution gradient is:
。
10. the method for identifying bitter components in a ginseng extract according to claim 8, wherein: in the step (5), the relative error of the peak time of the standard substance and the sample with the bitter value more than 0.8 is not more than 3 percent.
CN202310270868.2A 2023-03-20 2023-03-20 Preparation method of low-bitterness ginseng extract and identification method of bitter component in ginseng extract Pending CN116584649A (en)

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