CN114965802A - Quality control method of climacteric syndrome-relieving tablet - Google Patents

Quality control method of climacteric syndrome-relieving tablet Download PDF

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CN114965802A
CN114965802A CN202111524789.7A CN202111524789A CN114965802A CN 114965802 A CN114965802 A CN 114965802A CN 202111524789 A CN202111524789 A CN 202111524789A CN 114965802 A CN114965802 A CN 114965802A
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CN114965802B (en
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李运莉
薛欢鸽
梁雅芬
曹建军
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Yabao Pharmaceutical Group Corp
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    • 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
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Abstract

The invention relates to medicine detection, in particular to a high performance liquid chromatography fingerprint of a climacteric syndrome tablet and establishment of the fingerprint. The reference substance adopted by the detection method is 2,3,5,4' -tetrahydroxystilbene-2-O-beta-D-glucoside, and the high performance liquid chromatography analysis is carried out, wherein the chromatographic conditions are that octadecylsilane chemically bonded silica is used as a filling agent; the detection wavelength is 260-296 nm; taking methanol as mobile phase A and 0.1% phosphoric acid solution as mobile phase B, performing gradient elution at flow rate of 0.8-1.2ml/min and column temperature of 20-30 deg.C. The method can ensure the stability, consistency and controllability of the quality of the traditional Chinese medicine tablet, thereby ensuring the safety and effectiveness of the medicine.

Description

Quality control method of climacteric syndrome-relieving tablet
Technical Field
The invention relates to the field of medicine detection, in particular to a quality control method of a climacteric syndrome relieving tablet, and more particularly relates to high performance liquid chromatography fingerprint detection and fingerprint establishment of the climacteric syndrome relieving tablet.
Background
The climacteric syndrome relieving medicine is prepared with 15 kinds of Chinese medicinal materials including fleeceflower root, vine of multiflower knotweed, prepared rehmannia root, schisandra, oriental water plantain rhizome, tree peony bark, hooked uncaria, figwort, tuckahoe, curculigo rhizome, ophiopogon root, light wheat, magnetite, nacre and other material and through decoction, diacolation, concentration and other steps. The existing quality detection standard aims at the content of emodin to evaluate the quality of gengnian An, but the prepared polygonum multiflorum and the vine of multiflower knotweed in the prescription are two medicines which play a main role in gengnian An. The effective components of the two are 2,3,5,4' -tetrahydroxystilbene-2-O-beta-D-glucoside. There have been studies on the determination of the contents of 6 active ingredients in climacteric-syndrome for both (HPLC-DAD method for simultaneously determining the contents of 6 active ingredients in climacteric-syndrome, application method, etc., drug analysis of impurities 2012,32(1)), but this method employs 6 detection wavelengths for the 6 ingredients to measure separately, and is complicated.
The traditional Chinese medicine fingerprint is a comprehensive and quantifiable traditional Chinese medicine quality control means established on the basis of the research of a traditional Chinese medicine chemical component system, can describe and evaluate the quality of the traditional Chinese medicine on the whole, and has the characteristics of large information amount, strong characteristics, integrity and the like. At the present stage, under the condition that most of the effective components of the traditional Chinese medicine are not clear, the fingerprint spectrum can comprehensively reflect the relative relationship of the chemical components contained in the medicine, reflects the complexity and the correlation of the components of the traditional Chinese medicine, is adaptive to the traditional theory of the traditional Chinese medicine, can really and effectively characterize, comprehensively evaluate and comprehensively control the internal quality of the traditional Chinese medicine, and has important significance for effectively controlling the quality of the traditional Chinese medicine or the Chinese patent medicine.
Disclosure of Invention
The invention provides a fingerprint spectrum measuring method of climacteric syndrome relieving tablets, which can ensure the stability, consistency and controllability of the quality of the traditional Chinese medicine tablets, thereby ensuring the safety and effectiveness of the medicine.
In order to achieve the above object, the present invention provides a method for measuring a fingerprint of a climacteric syndrome tablet, comprising the steps of:
(1) preparation of reference solutions
Precisely weighing 2,3,5,4' -tetrahydroxystilbene-2-O-beta-D-glucoside reference substance, and dissolving in methanol to obtain reference solution;
(2) preparation of test solution
Removing coating from the climacteric syndrome relieving tablet, grinding, adding methanol solution, heating under reflux, and filtering to obtain filtrate.
(3) Measurement of
And sucking the reference substance solution and the test solution, and performing high performance liquid chromatography, wherein the chromatographic conditions are as follows:
octadecylsilane chemically bonded silica is used as a filling agent; the detection wavelength is 260-296 nm; taking methanol as mobile phase A and 0.1% phosphoric acid solution as mobile phase B, performing gradient elution at flow rate of 0.8-1.2ml/min and column temperature of 20-30 deg.C.
In one embodiment of the fingerprint determination method of the present invention, wherein the gradient program in step (3) is:
Figure BDA0003409788580000021
in one embodiment of the fingerprint measuring method of the present invention, the detection wavelength in the step (3) is 270 nm.
In one embodiment of the fingerprint measuring method of the present invention, the column temperature in the step (3) is 20 ℃.
The invention also provides a climacteric syndrome tablet fingerprint spectrum establishing method, which comprises the following steps:
(1) preparation of reference solutions
Accurately weighing 2,3,5,4' -tetrahydroxystilbene-2-O-beta-D-glucoside reference substance, and dissolving in methanol to obtain reference solution;
(2) preparation of test solution
Removing coating from the climacteric tablet, grinding, adding methanol solution, heating under reflux, filtering, and collecting the filtrate.
(3) Obtaining a chromatogram
And sucking the reference substance solution and the test solution, and performing high performance liquid chromatography, wherein the chromatographic conditions are as follows:
octadecylsilane chemically bonded silica is used as a filling agent; the detection wavelength is 260-296 nm; using methanol as mobile phase A and 0.1% phosphoric acid solution as mobile phase B, performing gradient elution at flow rate of 0.8-1.2ml/min and column temperature of 20-30 deg.C, and performing the following gradient:
Figure BDA0003409788580000022
(4) generating a comparison fingerprint
Selecting qualified chromatograms of a plurality of batches of the climacteric syndrome tablets, and taking a 2,3,5,4 '-tetrahydroxystilbene-2-O-beta-D-glucoside peak as a reference peak to obtain 10 maps with common peaks, wherein the retention time of the 2,3,5,4' -tetrahydroxystilbene-2-O-beta-D-glucoside is 55.2min, the retention time of harpagoside is 92.2min, the retention time of schisandrin is 101.5min, the retention time of deoxyschizandrin is 122.6min, the retention time of schisandrin is 128.1min, the retention time of curculigoside is 56.9min, and the relative retention time of the 10 common peaks is as follows:
Figure BDA0003409788580000031
in one embodiment of the present invention, the climacteric syndrome fingerprint establishing method, wherein the detection wavelength in step (3) is 270 nm.
In a specific embodiment of the climacteric syndrome tablet fingerprint spectrum establishing method, the column temperature in the step (3) is 20 ℃.
The invention establishes a fingerprint spectrum detection method of the preparation aiming at the problems of various medicinal herbs, complex components and difficulty in comprehensively reflecting the comprehensive information of the medicine by qualitative and quantitative analysis of individual components, so as to better and more effectively control the quality of the climacteric syndrome treating tablet.
Drawings
FIG. 1: finger print using mobile phase system 1
FIG. 2: finger print using mobile phase system 2
FIG. 3: finger print using mobile phase system 3
FIG. 4: finger print using mobile phase system 4
FIG. 5: finger print using mobile phase system 5
FIG. 6: fingerprint obtained by ultrasonic extraction or reflux extraction of test sample
FIG. 7: fingerprint obtained under different extraction solvents
FIG. 8: finger print at different column temperatures
FIG. 9: fingerprint for collecting chromatographic information within 140min
FIGS. 10-1 to 10-6 are fingerprints of 2,3,5,4' -tetrahydroxystilbene-2-O-beta-D-glucoside, harpagoside, schizandrin A, schizandrin B and curculigoside as reference substances for component identification, respectively.
FIGS. 10-7: test sample map
FIG. 11: and (4) fitting multiple batches of samples to the generated control fingerprints.
Detailed Description
EXAMPLE 1 selection of detection wavelength
Firstly, a DAD detector is adopted to detect a sample to be detected, the chromatographic peak information of the sample is inspected, and the detection wavelength is screened.
Preparation of a test solution: taking 20 tablets of the product, removing the coating, grinding, taking 3g, precisely weighing, placing in a conical flask with a plug, precisely adding 25ml of 75% methanol, sealing the plug, weighing, carrying out ultrasonic treatment (power 250W and frequency 40kHz) for 30 minutes, cooling, weighing again, supplementing the weight loss with 75% methanol, shaking up, filtering, and taking the subsequent filtrate to obtain the product.
By using
Figure BDA0003409788580000041
ODS-4 column, column temperature 30 deg.C, flow rate 0.8ml/min, acetonitrile as mobile phase A, aqueous solution as mobile phase B, gradient elution was performed as follows. Injecting sample 10ul, collecting time 150min,
Figure BDA0003409788580000042
the prescription of climacteric syndrome-relieving tablet contains 12 medicinal materials of rehmannia root, vine of multiflower knotweed, prepared fleece-flower root, etc., and its quality control components are vine of multiflower knotweed and prepared fleece-flower root, respectively, and their maximum absorption is 270-330 nm. The sample has rich chromatographic absorption in the wave band of 260nm-296nm, and compared with chromatographic peak conditions of the sample at 260nm, 270nm, 280nm and 296nm, the information content of the 270nm fingerprint spectrum is more, so that the chemical components of the product can be more fully embodied, the baseline drift is not large, the other medicinal material components have absorption at 270nm, and 270nm is selected as the detection wavelength.
Example 2 mobile phase System selection
Preparation of a test solution: taking 20 tablets of the product, removing the coating, grinding, taking 3g, precisely weighing, placing in a conical flask with a plug, precisely adding 25ml of 75% methanol, sealing the plug, weighing, carrying out ultrasonic treatment (power 250W and frequency 40kHz) for 30 minutes, cooling, weighing again, supplementing the weight loss with 75% methanol, shaking up, filtering, and taking the subsequent filtrate to obtain the product.
By using
Figure BDA0003409788580000051
ODS-4 column (250 mm. times.4.6 mm, 5 μm) was tested by examining acetonitrile-0.05% phosphoric acid solution, methanol-0.1% phosphoric acid solution and the like.
(1) The system 1:
acetonitrile is used as mobile phase A, 0.05% phosphoric acid solution is used as mobile phase B, the collection time is 50min, the elution gradient is shown in the following table, and the result is shown in figure 1.
Figure BDA0003409788580000052
(2) And (3) system 2: acetonitrile is used as mobile phase A, 0.05% phosphoric acid solution is used as mobile phase B, the collection time is 140min, the elution gradient is shown in the following table, and the result is shown in figure 2.
Figure BDA0003409788580000053
(3) And (3) system: methanol is used as mobile phase A, 0.1% phosphoric acid solution is used as mobile phase B, the collection time is 140min, the elution gradient is shown in the following table, and the result is shown in figure 3.
Figure BDA0003409788580000054
(4) And (4) system: methanol is used as mobile phase A, 0.1% phosphoric acid solution is used as mobile phase B, the collection time is 140min, the elution gradient is shown in the following table, and the result is shown in figure 4.
Figure BDA0003409788580000055
Figure BDA0003409788580000061
(5) And (5) the system: methanol is used as mobile phase A, 0.1% phosphoric acid solution is used as mobile phase B, the collection time is 140min, the elution gradient is shown in the following table, and the result is shown in figure 5.
Figure BDA0003409788580000062
As can be seen from the above experiment, the methanol-0.1% phosphoric acid solution system (system 5) has the best separation effect on the chromatographic peak of the test solution of the climacteric syndrome tablet, the peak shape is good, the base line is stable, and the required separation degree is achieved.
Example 3 examination of extraction mode
Taking 20 tablets of the product, removing the coating, grinding, taking 3g, precisely weighing, placing in a conical flask with a plug, precisely adding 20ml of methanol, sealing the plug, weighing, carrying out ultrasonic treatment (power 250W and frequency 40kHz) for 1 hour, cooling, weighing again, supplementing the weight loss by using methanol, shaking up, filtering, and taking the subsequent filtrate.
Taking 20 tablets of the product, removing the coating, grinding, taking 3g, precisely weighing, placing in a conical flask with a plug, precisely adding 20ml of methanol, sealing the plug, weighing, heating and refluxing for 1 hour, cooling, weighing again, supplementing the lost weight with methanol, shaking uniformly, filtering, and taking the subsequent filtrate.
Measuring by high performance liquid chromatography (China pharmacopoeia 2020 edition four-part general regulation 0512).
Octadecylsilane chemically bonded silica is used as filler (
Figure BDA0003409788580000063
ODS-4 column, 250mm in length, 4.6mm in inner diameter, S/N7 AF37032), using methanol as mobile phase A and 0.1% phosphoric acid solution as mobile phase B, and performing gradient elution according to the following table; the flow rate is 1.0 ml/min; the detection wavelength is 270 nm; the column temperature was 25 ℃.
Figure BDA0003409788580000064
Precisely sucking 10 μ l of each sample solution, injecting into liquid chromatograph, and measuring. The results are shown in the following table and FIG. 6.
Figure BDA0003409788580000071
As can be seen from the above table, when the reflux extraction is adopted, the amount of the obtained fingerprint information is large, and the peak response value is large, so the reflux extraction is adopted.
Example 4 extraction solvent examination
Taking 20 tablets of the product, removing the coating, grinding, taking 3g, precisely weighing, placing in a conical flask with a plug, precisely adding 20ml of water, 25% methanol, 50% methanol, 75% methanol, methanol and absolute ethanol respectively, sealing the plug, weighing, heating and refluxing for 1 hour, cooling, weighing again, supplementing the lost weight with water, 25% methanol, 50% methanol, 75% methanol, methanol and absolute ethanol respectively, shaking up, filtering, and taking the subsequent filtrate to obtain the product.
The measurement method was the same as in example 3. The results are shown in the following table, FIG. 7.
Figure BDA0003409788580000072
Figure BDA0003409788580000081
EXAMPLE 5 examination of column temperature
In the chromatographic fingerprint detection, the column temperature usually affects the separation effect, and the inventor analyzes the fingerprint of the test solution of the climacteric syndrome tablet under the three column temperature conditions of 20 ℃, 25 ℃ and 30 ℃. Other conditions were as in example 8. The result shows that the chromatographic peak separation effect is good and the baseline is stable at 20 ℃, so the column temperature at the time of detection is optimally selected to be 20 ℃. See fig. 8.
Example 6 chromatographic information acquisition time determination
The reference solution and the test solution were prepared as in example 8. In order to investigate the chromatographic information acquisition time, the product is detected under the following chromatographic conditions: the chromatographic column is as follows:
Figure BDA0003409788580000082
ODS-4 column (250 mm. times.4.6 mm, 5 μm); the detection wavelength is 270 nm; the column temperature is 20 ℃; the flow rate is 1.0 ml/min; the sample amount is 10 mul; mobile phase: gradient elution was performed according to the following table using methanol as mobile phase a and 0.1% phosphoric acid solution as mobile phase B. The result is shown in figure 9, no chromatographic peak is present after 140min, so only the chromatographic information within 140min is collected.
Figure BDA0003409788580000083
Figure BDA0003409788580000091
EXAMPLE 7 selection of reference
The reference solution and the sample solution were prepared and the chromatographic conditions were the same as in example 8. According to the chemical components contained in the medicinal materials of GENGNIANAN tablet, 2,3,5,4' -tetrahydroxystilbene-2-O-beta-D-glucoside, harpagoside, schizandrin, deoxyschizandrin, schisandrin B and curculigoside are selected as reference substances for component confirmation, and the results are shown in figures 10-1 to 10-7.
As can be seen from comparison of the test sample fingerprint and the control sample fingerprint, the retention time of 2,3,5,4' -tetrahydroxystilbene-2-O-beta-D-glucoside is 55.2min, the retention time of harpagoside is 92.2min, the retention time of schizandrol A is 101.5min, the retention time of deoxyschizandrin is 122.6min, the retention time of schisandrin B is 128.1min, and the retention time of curculigoside is 56.9 min. The ratio of the peak area of the 2,3,5,4 '-tetrahydroxystilbene-2-O-beta-D-glucoside chromatographic peak in the fingerprint of the test sample is relatively large, and the result of the actual measurement of a plurality of samples shows that the peak area is relatively stable, so that the 2,3,5,4' -tetrahydroxystilbene-2-O-beta-D-glucoside is selected as a reference peak and is used as a reference object of the climacteric syndrome fingerprint.
Example 8 Gengnian comparison fingerprint establishment
Preparation of reference solutions: accurately weighing 10mg of 2,3,5,4' -tetrahydroxystilbene-2-O-beta-D-glucoside reference substance, placing the reference substance in a 200ml brown measuring flask, adding methanol to dissolve and dilute the reference substance to a scale, and shaking up to obtain the product. (50. mu.g of solution per 1 ml)
Preparation of a test solution: taking 20 tablets of the product, removing the coating, grinding, taking 3g, precisely weighing, placing in a conical flask with a plug, precisely adding 20ml of methanol, sealing the plug, weighing, heating and refluxing for 30 minutes, cooling, weighing again, supplementing the lost weight with methanol, shaking uniformly, filtering, and taking the subsequent filtrate.
Chromatographic conditions and system applicability test: measuring by high performance liquid chromatography (China pharmacopoeia 2020 edition four-part general regulation 0512). Octadecylsilane chemically bonded silica was used as a filler (column:
Figure BDA0003409788580000092
ODS-4250 mm. times.4.6 mm, 5 μm); the detection wavelength is 270 nm; the column temperature is 20 ℃; the flow rate is 1.0 ml/min; gradient elution was performed according to the following table using methanol as mobile phase a and 0.1% phosphoric acid solution as mobile phase B. The number of theoretical plates is not less than 10000 in terms of 2,3,5,4' -tetrahydroxystilbene-2-O-beta-D-glucoside peak. Are respectively provided withPrecisely sucking 10 μ l of each of the reference solution and the sample solution, injecting into a liquid chromatograph, measuring, and recording chromatogram for 140 minutes.
Figure BDA0003409788580000093
Figure BDA0003409788580000101
The batch numbers of 201101, 201102, 201103, 201104, 201201, 201202, 201203, 201204, 201205 and 201206 climacteric syndrome tablets produced by Yabao pharmaceutical industry group Limited company are respectively detected according to the established fingerprint spectrum measuring method, a national pharmacopoeia Committee's traditional Chinese medicine chromatogram fingerprint spectrum similarity evaluation system' (version 2012.130723) is adopted to fit and generate a comparison fingerprint spectrum, which is shown in figure 11, and 2,3,5,4 '-tetrahydroxy stilbene-2-O-beta-D-glucoside peak is taken as a reference peak to obtain 10 spectrums with common peaks, wherein the retention time of 2,3,5,4' -tetrahydroxy stilbene-2-O-beta-D-glucoside is 55.2min, the retention time of harpagoside is 92.2min, the retention time of schisandrin is 101.5min, the retention time of deoxyschizandrin is 122.6min, and the retention time of schisandrin is 122.6min, The retention time of schisandrin B is 128.1min, the retention time of curculigoside is 56.9min, and the relative retention time of 10 common peaks is as follows:
Figure BDA0003409788580000102

Claims (7)

1. a fingerprint spectrum measuring method of climacteric syndrome-relieving tablets comprises the following steps:
(1) preparation of reference solutions
Precisely weighing 2,3,5,4' -tetrahydroxystilbene-2-O-beta-D-glucoside reference substance, and dissolving in methanol to obtain reference solution;
(2) preparation of test solution
Taking the climacteric syndrome relieving tablet, removing coating, grinding, adding methanol solution, heating under reflux for extraction, filtering, and collecting filtrate;
(3) measurement of
And sucking the reference substance solution and the test solution, and performing high performance liquid chromatography, wherein the chromatographic conditions are as follows:
octadecylsilane chemically bonded silica is used as a filling agent; the detection wavelength is 260-296 nm; taking methanol as mobile phase A and 0.1% phosphoric acid solution as mobile phase B, performing gradient elution at flow rate of 0.8-1.2ml/min and column temperature of 20-30 deg.C.
2. The fingerprint determination method according to claim 1, wherein said gradient program in step (3) is:
Figure FDA0003409788570000011
3. the fingerprint measuring method according to claim 1, wherein the detection wavelength in said step (3) is 270 nm.
4. The fingerprint measuring method according to claim 1 wherein the column temperature in said step (3) is 20 ℃.
5. A climacteric syndrome tablet fingerprint establishing method comprises the following steps:
(1) preparation of reference solutions
Precisely weighing 2,3,5,4' -tetrahydroxystilbene-2-O-beta-D-glucoside reference substance, and dissolving in methanol to obtain reference solution;
(2) preparation of test solution
Removing coating from the climacteric tablet, grinding, adding methanol solution, heating under reflux, and filtering to obtain filtrate;
(3) obtaining the chromatogram
And (3) sucking the reference substance solution and the test solution, and performing high performance liquid chromatography analysis under the following chromatographic conditions:
octadecylsilane chemically bonded silica is used as a filling agent; the detection wavelength is 260-296 nm; using methanol as mobile phase A and 0.1% phosphoric acid solution as mobile phase B, performing gradient elution at flow rate of 0.8-1.2ml/min and column temperature of 20-30 deg.C, and performing the following gradient:
Figure FDA0003409788570000021
(4) generating a comparison fingerprint
Selecting qualified chromatograms of a plurality of batches of the climacteric syndrome tablets, and taking a 2,3,5,4 '-tetrahydroxystilbene-2-O-beta-D-glucoside peak as a reference peak to obtain 10 maps with common peaks, wherein the retention time of the 2,3,5,4' -tetrahydroxystilbene-2-O-beta-D-glucoside is 55.2min, the retention time of harpagoside is 92.2min, the retention time of schisandrin is 101.5min, the retention time of deoxyschizandrin is 122.6min, the retention time of schisandrin is 128.1min, the retention time of curculigoside is 56.9min, and the relative retention time of the 10 common peaks is as follows:
Figure FDA0003409788570000022
6. the method of establishing a fingerprint according to claim 5 wherein the detection wavelength in step (3) is 270 nm.
7. The fingerprint measuring method according to claim 5 wherein the column temperature in step (3) is 20 ℃.
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Publication number Priority date Publication date Assignee Title
CN116165320A (en) * 2023-04-21 2023-05-26 保定市食品药品检验所 Traditional Chinese medicine fingerprint detection method of blood-nourishing nerve-soothing tablet
CN116165320B (en) * 2023-04-21 2023-07-21 保定市食品药品检验所 Traditional Chinese medicine fingerprint detection method of blood-nourishing nerve-soothing tablet

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