CN112730698A - Content determination method of traditional Chinese medicine preparation for treating depression - Google Patents
Content determination method of traditional Chinese medicine preparation for treating depression Download PDFInfo
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- CN112730698A CN112730698A CN202110149706.4A CN202110149706A CN112730698A CN 112730698 A CN112730698 A CN 112730698A CN 202110149706 A CN202110149706 A CN 202110149706A CN 112730698 A CN112730698 A CN 112730698A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/14—Preparation by elimination of some components
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/36—Control of physical parameters of the fluid carrier in high pressure liquid systems
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/50—Conditioning of the sorbent material or stationary liquid
- G01N30/52—Physical parameters
- G01N30/54—Temperature
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/74—Optical detectors
Abstract
The invention relates to a content determination method of a traditional Chinese medicine preparation for treating depression, and establishes an HPLC content determination method for simultaneously determining the content of 3 components of syringin, geniposide and schizandrol A in the traditional Chinese medicine preparation for treating depression.
Description
One, the technical field
The invention relates to the technical field of traditional Chinese medicines, in particular to a content determination method of a traditional Chinese medicine preparation for treating depression.
Second, background Art
The preparation is a novel traditional Chinese medicine preparation, and has the main functions of: tonify kidney, regulate qi, relieve depression and induce tranquilization. Can be used for treating depression caused by kidney essence deficiency and stagnation of liver-qi. The preparation is prepared by extracting and concentrating acanthopanax, radix curcumae, schisandra and gardenia, adding a proper amount of auxiliary materials, preparing into granules and packaging.
Journal literature (Zhao Weiyun, Sun Yanzhi, Gao Song, etc. RP-HPLC method for simultaneously determining geniposide and schisandrin [ J ] in Yinaojieyu granules. research and development of natural products. 2015,27: 1215-.
Third, the invention
The invention aims to overcome the defects in the prior art and provide a method for controlling the overall quality of the preparation so as to better control the quality of the preparation.
The invention provides an HPLC content determination method for simultaneously determining the content of 3 components of syringin, geniposide and schizandrin in a traditional Chinese medicine preparation for treating depression.
The traditional Chinese medicine preparation for treating depression is prepared from the following raw materials, by weight, 20-40 parts of acanthopanax, 10-30 parts of radix curcumae, 5-15 parts of schisandra and 4-12 parts of cape jasmine.
The pharmaceutical composition can be prepared into granules, tablets, capsules and the like according to a conventional pharmaceutical method.
The content determination method of the invention aims at various pharmaceutical composition preparations which are prepared by taking 20-40 parts by weight of acanthopanax, 10-30 parts by weight of radix curcumae, 5-15 parts by weight of schisandra and 4-12 parts by weight of gardenia as raw materials, and the equivalent crude drug content of each preparation taken every day is the same.
The content determination and detection method comprises the following steps:
in the detection process, the preparation is prepared into a solution to be detected according to the following method: taking a proper amount of the product, grinding, taking about 0.5-1.5g, precisely weighing, placing in a conical flask with a plug, precisely adding 50ml of methanol, weighing, carrying out ultrasonic treatment for 30 minutes, cooling, weighing again, supplementing the lost weight with methanol, shaking uniformly, filtering, taking the subsequent filtrate, and measuring.
The preparation method of the mixed reference substance in the detection process comprises the following steps: taking a proper amount of syringin, geniposide and schizandrol A reference substances, precisely weighing, and adding methanol to prepare a solution containing 9 μ g of syringin, 250 μ g of geniposide and 16 μ g of schizandrol A per 1 ml.
The determination method comprises the following steps: precisely sucking 10 μ l of each of the reference solution and the sample solution, injecting into a liquid chromatograph, and performing gradient elution as follows:
wherein the mobile phase A is methanol, and the mobile phase B is water or 0.1 percent phosphoric acid solution. The gradient elution procedure was:
the detection wavelength is 265nm in 0-20 min, 238nm in 20-35 min and 250nm in 35-60 min. Column temperature: 30 ℃, flow rate 1.0ml/ml, sample size 10 μ, column: c18 chromatography column.
The quality detection method as described above may include the steps of:
preparation of a test solution: taking a proper amount of the product, grinding, precisely weighing about 1g, placing into a conical flask with a plug, precisely adding 50ml of methanol, weighing, ultrasonically treating for 30 minutes, cooling, weighing again, supplementing the lost weight with methanol, shaking up, filtering, and taking the subsequent filtrate.
Preparation of control solutions: taking a proper amount of syringin, geniposide and schizandrol A reference substances, precisely weighing, and adding methanol to prepare a solution containing 9 μ g of syringin, 250 μ g of geniposide and 16 μ g of schizandrol A per 1 ml.
Precisely sucking 10 μ l of each of the reference solution and the sample solution, injecting into a liquid chromatograph, and performing gradient elution as follows:
wherein the mobile phase A is methanol, and the mobile phase B is water or 0.1 percent phosphoric acid. The detection wavelength is 265nm in 0-20 min, 238nm in 20-35 min and 250nm in 35-60 min.
The detection wavelength is 265nm in 0-20 min, 238nm in 20-35 min and 250nm in 35-60 min. Column temperature: 30 ℃, flow rate 1.0ml/ml, sample size 10 μ, column: c18 chromatography column.
The method simultaneously determines the content of index components in the three medicinal materials in the formula, has simple, convenient, sensitive and quick operation, and can well control the quality of products.
Description of the drawings
FIG. 1 is a chromatogram of a negative interference test without Acanthopanax senticosus, Gardenia jasminoides ellis and Schisandra chinensis.
Fifth, detailed description of the invention
The invention will now be further illustrated by reference to specific examples, which are intended to be illustrative only and not to limit the scope of the invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
Example 1
(1) Instrument and reagent
Waters2695-2998 high performance liquid chromatography (Waters corporation), ultrasonic cleaner (KQ-500DE type); methanol (chromatographically pure); syringin, geniposide and schizandrol A reference substances are purchased from China food and drug testing research institute; the preparation is prepared by Zhongjingzuoxi pharmaceutical corporation.
(2) Chromatographic conditions
The mobile phase A is methanol, the mobile phase B is water or 0.1 percent phosphoric acid, and the mobile phase gradient is as follows:
detection wavelength: 265nm in 0-20 min, 238nm in 20-35 min and 250nm in 35-60 min; a chromatographic column: a C18 chromatography column; flow rate: 1.0 ml/min; column temperature: and (4) room temperature.
(3) System suitability test
Under the chromatographic condition, the peak separation effect of the syringin, the geniposide, the schizandrol A and other impurities is better, and the theoretical plate number is not less than 2000 calculated according to the syringin.
(4) Extraction solvent, extraction method and selection of extraction time
Through experiments, the sample extraction solvent is methanol, the extraction method is ultrasonic, and the extraction time is 30 minutes.
(5) Preparation of reference solution and test solution
Preparation of control solutions: taking a proper amount of syringin, geniposide and schizandrol A reference substances, precisely weighing, and adding methanol to prepare a solution containing 9 μ g of syringin, 250 μ g of geniposide and 16 μ g of schizandrol A per 1 ml.
II, preparing a test solution: preparation of a test solution: taking a proper amount of the product, grinding, precisely weighing about 1g, placing into a conical flask with a plug, precisely adding 50ml of methanol, weighing, ultrasonically treating for 30 minutes, cooling, weighing again, supplementing the lost weight with methanol, shaking up, filtering, and taking the subsequent filtrate.
III, preparation of negative control solution: preparing 1g of three negative samples which do not contain acanthopanax, gardenia and schisandra respectively, and preparing negative control solutions for later use by the same method.
(6) Negative interference test
Precisely sucking 10 μ l of each of the test solution, the negative control solution and the reference substance, injecting into a liquid chromatograph, and determining by the chromatogram that at the position with the same retention time as the reference substance chromatographic peak, chromatographic peaks with the same retention time of the test solution appear, and each negative control solution has no absorption at the wavelength, and has no interference on the content determination of syringin, geniposide and schizandrin A, as shown in figure 1.
(7) Investigation of linear relationships
The experimental result shows that the syringin has good linear relation in the range of 1.2269-15.3358 mug/ml; the linear relation of the geniposide is good in the range of 59.9846-749.8080 mu g/ml; schizandrol A has good linear relationship in the range of 2.8388-35.4845 μ g/ml.
(8) Precision test
The experimental result shows that the RSD is less than 2 percent, which indicates that the precision is good.
(9) Stability test
The results show that the test solution was stable for 28 hours.
(10) Repeatability test
The experimental result shows that RSD is less than 2 percent, which indicates that the method has good repeatability.
(11) Recovery test
The results show that the syringin recovery rate is in the range of 90-108%, the geniposide recovery rate is in the range of 92-105%, and the schizandrol A recovery rate is in the range of 90-108%, which indicates that the determination method is feasible.
(12) Determination of sample content
Example 2
Extracting radix Acanthopanacis Senticosi, radix Curcumae, fructus Schisandrae chinensis, and fructus Gardeniae, concentrating, adding appropriate amount of adjuvants, granulating, and packaging.
The content determination method comprises the following steps:
octadecylsilane chemically bonded silica is used as a filler in chromatographic conditions and system applicability tests; gradient elution is carried out by taking methanol as a mobile phase A and water as a mobile phase B according to the specification in the following table, wherein the gradient elution is carried out for 0-20 min at 265nm, for 20-35 min at 238nm and for 35-60 min at 250 nm. The number of theoretical plates is not less than 2000 calculated according to syringin peak.
Preparation of control solutions: taking a proper amount of syringin, geniposide and schizandrol A reference substances, precisely weighing, and adding methanol to prepare a solution containing 9 μ g of syringin, 250 μ g of geniposide and 16 μ g of schizandrol A per 1 ml.
Preparation of a test solution: taking the product, grinding, weighing about 1g, precisely weighing, placing in a conical flask with a plug, precisely adding 50ml of methanol, weighing, ultrasonically treating for 30 minutes, cooling, weighing again, supplementing the weight loss with methanol, shaking up, filtering, and taking the subsequent filtrate.
The determination method comprises the following steps: precisely sucking 10 μ l of each of the reference solution and the sample solution, injecting into liquid chromatograph, and measuring.
The above description is only a preferred embodiment of the present invention, and several modifications and additions may be made without departing from the method of the present invention, which should also be considered as the protection scope of the present invention.
Claims (4)
1. A content determination method of a traditional Chinese medicine preparation for treating depression is characterized by comprising the following steps:
(1) preparing a test sample: taking a proper amount of the product, grinding, taking about 0.5-1.5g, precisely weighing, placing in a conical flask with a plug, precisely adding 50ml of methanol, weighing, carrying out ultrasonic treatment for 30 minutes, cooling, weighing again, supplementing the lost weight with methanol, shaking up, filtering, and taking a subsequent filtrate to obtain a test solution;
(2) preparation of mixed control solution: taking a proper amount of syringin, geniposide and schizandrol A reference substances, precisely weighing, and adding methanol to obtain a mixed reference substance solution;
(3) the determination method comprises the following steps: precisely sucking 10 μ l of each of the reference solution and the sample solution, injecting into a liquid chromatograph, and performing gradient elution as follows:
wherein the mobile phase A is methanol, and the mobile phase B is water or 0.1 percent phosphoric acid solution. The gradient elution procedure was:
the detection wavelength is 265nm in 0-20 min, 238nm in 20-35 min and 250nm in 35-60 min. Column temperature: 30 ℃, flow rate 1.0ml/ml, sample size 10 μ, column: c18 chromatography column.
2. The method for measuring the content of the traditional Chinese medicine preparation for treating depression according to claim 1, wherein the concentration of each component of the mixed control solution in the step (2) is 9 μ g of syringin, 250 μ g of geniposide and 16 μ g of schizandrin in each 1 ml; the regression equation for measuring the syringin content is good in linear relation in the range of 1.2269-15.3358 mu g/ml; the regression equation for determining the content of the geniposide has good linear relation in the range of 59.9846-749.8080 mu g/ml; the regression equation for measuring the content of the schizandrol A has good linear relation in the range of 2.8388-35.4845 mu g/ml.
3. The method for measuring the content of the traditional Chinese medicine preparation for treating depression according to claim 1, wherein the preparation of the test sample in the step (1) can be realized by the following method: taking a proper amount of the product, grinding, precisely weighing about 1g, placing into a conical flask with a plug, precisely adding 50ml of methanol, weighing, ultrasonically treating for 30 minutes, cooling, weighing again, supplementing the lost weight with methanol, shaking up, filtering, and taking the subsequent filtrate.
4. The content determination method of the traditional Chinese medicine preparation for treating depression according to claim 1, characterized in that the traditional Chinese medicine preparation is prepared from the following traditional Chinese medicine compositions in parts by weight: 20-40 parts of acanthopanax, 10-30 parts of radix curcumae, 5-15 parts of schisandra and 4-12 parts of gardenia.
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