CN109540896B - Quality control method of traditional Chinese medicine capsule with liver injury protection function - Google Patents
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Abstract
The invention discloses a quality control method of a traditional Chinese medicine capsule with a liver injury protection function, which adopts three methods of microscopic identification, thin-layer identification and quantitative determination of functional components to carry out quality control: 1) microscopic identification: the contents of the product are taken, treated and observed under a microscope, and thin and light brown hyphae are scattered and distributed in a curved shape, are few branched and have the diameter of about 3 to 7 micrometers. 2) Thin-layer identification: in the chromatogram of the test solution, the same brown spots appear in the sunlight at the corresponding positions of the chromatogram of the radix astragali control solution; the same orange-yellow fluorescent spots are displayed under an ultraviolet lamp (365 nm); 3) quantitative determination of functional components: the effective component schizandrol A in the capsule is determined by high performance liquid chromatography, and the content of the capsule per gram contains fructus Schisandrae calculated as schizandrol A, and is not less than 0.5 mg. The method has the advantages of good stability, good repeatability, high recovery rate and strong specificity. The invention improves the quality standard of a traditional Chinese medicine capsule with auxiliary protection function on liver injury.
Description
Technical Field
The invention relates to the field of traditional Chinese medicines, in particular to a quality control method of a traditional Chinese medicine capsule with a function of protecting liver injury.
Background
A Chinese medicine in the form of capsule for helping to protect liver is prepared from six Chinese-medicinal materials including pueraria root, hovenia dulcis, astragalus root, ganoderma, schisandra fruit, galangal rhizome, etc through modern preparing process. Because the chemical components of the traditional Chinese medicine are complex and seriously interfere the qualitative and quantitative control process of the functional components of the traditional Chinese medicine preparation, in order to ensure that the quality of the traditional Chinese medicine capsule with the auxiliary protection function on liver injury is controllable and stable, the invention adopts three methods of microscopic identification, thin-layer identification and functional component content measurement to carry out qualitative and quantitative quality control, and is a quality control method with strong specificity, effectiveness and accuracy.
The invention firstly adopts a microscopic identification method to identify the lucid ganoderma sporocarp in the traditional Chinese medicine capsule with the auxiliary protection function on liver injury. The ganoderma lucidum fruiting body contains basic nutrients such as polysaccharide, vegetable protein and the like, and also contains various secondary metabolites such as triterpenes, adenosine, alkaloids and the like, and the main nutrients and functional components of the ganoderma lucidum are concentrated, but the ganoderma lucidum fruiting body is cultured by a solid culture method and a liquid fermentation method, because the solid culture time is longer than the liquid fermentation time, the differences of the nutrients and the functional components are obvious, particularly the triterpenes functional components, and the solid culture is obviously higher than the liquid fermentation time, the invention establishes a microscopic identification project aiming at the solid culture ganoderma lucidum fruiting body so as to control the quality of the traditional Chinese medicine capsule.
The invention adopts a thin-layer identification method to qualitatively identify the astragalus root and the functional component astragaloside in the capsule, because the prescription contains volatile oil grease compounds of galangal, in order to eliminate the interference of fat-soluble components and other impurities in the traditional Chinese medicine capsule on the identification process, refining and purifying steps such as ether degreasing, methanol extraction, n-butanol extraction, alkalization impurity removal, macroporous resin purification and the like are adopted, a thin-layer identification pretreatment method is established, finally, a lower layer solution of dichloromethane-methanol-water (12: 8: 3) is used as a developing agent to carry out thin-layer development, environment-friendly dichloromethane is selected to replace highly toxic trichloromethane, a thin-layer development system is established, and the established thin-layer identification method has strong specificity, effectiveness and accuracy.
The invention adopts high performance liquid chromatography to quantitatively determine the functional component schisandrin in the capsules. In order to eliminate the influence of the volatile oil fat-soluble ingredients on quantitative determination in the traditional Chinese medicine capsule, the diatomite is added in the process of extracting and enriching the functional ingredients for adsorbing the volatile oil fat-soluble ingredients, so that the interference of the ingredients on sample determination is reduced, and the specificity of quantitative determination can be well improved.
Disclosure of Invention
The invention aims to provide a quality control method of a traditional Chinese medicine capsule with a function of protecting liver injury, so that the quality of a product is better controlled. In order to realize the purpose, the invention adopts the following technical scheme: a quality control method of a traditional Chinese medicine capsule with a function of protecting liver injury is characterized in that three methods of microscopic identification, thin-layer identification and content measurement are adopted for quality control.
1) Microscopic identification: taking the content of the capsule, grinding the content, screening the content by a No. 5 sieve, selecting a proper amount of powder, placing the powder on a cover glass, dropwise adding a chloral hydrate test solution, covering the cover glass, and observing the content under a microscope: the thin, light brown hyphae are scattered, curved, and have few branches with a diameter of about 3 to 7 microns.
2) Thin-layer identification: taking capsule content, grinding, taking powder 12g, adding ether 60ml, shaking for 1 hour, filtering and discarding filtrate, using methanol 60ml for medicine residue, heating and refluxing for 1 hour, filtering, recovering solvent from filtrate until dry, adding water 30ml for dissolving residue, shaking and extracting for 4 times (20ml, 20ml, 15ml, 15ml) with water saturated n-butyl alcohol, combining n-butyl alcohol solution, washing with ammonia test solution, recovering solvent from n-butyl alcohol solution until dry, adding water 20ml for dissolving residue, cooling, passing through D101 type macroporous adsorbent resin column (column inner diameter is 1.5cm, column height is 15cm), eluting with water 40ml, discarding eluent, eluting with 40% ethanol 50ml, discarding eluent, then eluting with 70% ethanol 50ml, collecting eluent, recovering solvent until dry, adding methanol 1ml for dissolving residue to serve as test solution. Preparing another 3g of radix astragali, and preparing a reference medicinal solution by the same method. Adding methanol into astragaloside IV control to obtain 1mg solution per 1ml, and making into control solution. Absorbing 5-10 μ l of the above three solutions by thin layer chromatography, dropping on the same silica gel G thin layer plate, developing with dichloromethane-methanol-water (12: 8: 3) lower layer solution as developing agent, taking out, air drying, spraying with 10% sulfuric acid ethanol solution, and heating at 105 deg.C until the spots are clearly developed. The chromatogram of the test sample and the chromatogram of the reference sample are in corresponding positions, and the same brown spots appear in sunlight; the same orange-yellow fluorescent spots were shown under an ultraviolet lamp (365 nm).
3) The effective component schizandrol A in the capsule is determined by high performance liquid chromatography:
the preparation method of the reference solution comprises the following steps: precisely weighing appropriate amount of schizandrol A as reference substance, and adding methanol to obtain solution containing 0.15mg/mL of schizandrol A as reference substance solution.
The preparation method of the test solution comprises the following steps: taking about 4g of the content of the product, precisely weighing, adding 5g of diatomite, uniformly mixing, then placing in a Soxhlet extractor, adding 50mL of methanol, heating and refluxing for 4 hours, recovering the solvent from the extracting solution, concentrating to dryness, adding methanol to dissolve residues, transferring to a 25mL measuring flask, adding methanol to the scale, shaking uniformly, filtering with a 0.45um organic filter membrane, and taking the subsequent filtrate to obtain a sample solution.
The determination method comprises precisely sucking 10uL of each of the reference solution and the sample solution, injecting into a liquid chromatograph, and determining, wherein the chromatographic conditions are as follows: octadecylsilane chemically bonded silica is used as a filling agent; gradient elution with acetonitrile (A) -water (B) as mobile phase (0 min: 45% A → 25 min: 68% A → 40 min: 68% A → 60 min: 45% A) with detection wavelength of 250 nm; the theoretical plate number is not less than 3000 according to the peak value of schizandrol A; the content of the capsule per g contains fructus Schisandrae chinensis (calculated as schisandrin) not less than 0.5 mg.
The invention has the advantages that: the invention aims at a traditional Chinese medicine capsule with a function of protecting liver injury, and performs thin-layer identification of astragalus, liquid-phase identification of schisandrin of schisandra and liquid-phase identification of astragaloside IV of astragalus. The method has the advantages of good stability, good repeatability, high recovery rate and strong specificity. The method of the invention is used for detecting the traditional Chinese medicine capsule with the function of protecting liver injury, and improves the stability and controllability of the quality of the traditional Chinese medicine capsule with the function of protecting liver injury.
Drawings
FIG. 1 is a microscopic identification picture.
FIG. 2 is a thin layer chromatogram in sunlight.
FIG. 3 is a thin layer chromatogram under an ultraviolet lamp (365 nm): 1A Chinese medicinal capsule 00DJD01 with liver injury protecting effect; 2 radix astragali as reference material; 3 astragaloside IV reference substance; 4 a Chinese medicinal capsule 00DJD02 with the function of protecting liver injury.
FIG. 4 is a spectrum of a schizandrol A control substance in a Chinese medicinal capsule with liver injury protecting effect.
FIG. 5 is a schizandrol A spectrum of a Chinese medicinal capsule sample with liver injury protecting effect.
Detailed Description
EXAMPLE 1 microscopic identification
Taking the capsule content, grinding, sieving by a No. 5 sieve, selecting a proper amount of powder, placing on a cover glass, dropwise adding a chloral hydrate test solution, covering the cover glass, and observing under a microscope: the microscopic features are more apparent in the form of thin, light brown hyphae scattered, curved, and a few bifurcations, approximately 3 to 7 microns in diameter, (see FIG. 1), meeting the standard.
Example 2 thin layer identification
Taking capsule content, grinding to obtain powder 12g, adding diethyl ether 60ml, shaking for 1 hr, filtering to remove filtrate, extracting the residue with methanol 60ml, heating and refluxing for 1 hr, filtering, recovering solvent from the filtrate to dryness, adding water 30ml into the residue to dissolve, shaking and extracting with water saturated n-butanol for 4 times (20ml, 20ml, 15ml, 15ml), mixing n-butanol solutions, washing with ammonia test solution, recovering solvent from n-butanol solution to dryness, adding water 20ml into the residue to dissolve, cooling, passing through D101 type macroporous adsorbent resin column (column inner diameter is 1.5cm, column height is 15cm), eluting with water 40ml, discarding eluent, eluting with 40% ethanol 50ml, discarding eluent, eluting with 70% ethanol 50ml, collecting eluent, recovering solvent to dryness, adding methanol 1ml into the residue to dissolve, and using as test solution. Another 3g of radix astragali is prepared and used for preparing a control medicinal solution by the same method. Adding methanol into astragaloside IV control to obtain 1mg solution per 1ml as control solution. And performing thin layer chromatography by sucking 5-10 μ l of the above three solutions, respectively dropping on the same silica gel G thin layer plate, developing with dichloromethane-methanol-water (12: 8: 3) lower layer solution as developing agent, taking out, air drying, spraying 10% sulphuric acid ethanol solution, and heating at 105 deg.C until the spots are clearly developed.
The thin layer identifies that the chromatogram of the test sample and the chromatogram of the reference sample show the same tan spots in the sunlight at the corresponding positions; the same orange yellow fluorescent spots are displayed under an ultraviolet lamp (365nm), and the three batches of samples are detected to be in accordance with the standard.
(see FIGS. 2 and 3)
Example 3 quantitative determination of efficacy component
1, instrument and reagent:
agilent1200 high performance liquid chromatograph.
Ultrasonic cleaning machine (Power 200w, frequency 40KHz)
Electronic balance XS105 type
Acetonitrile is chromatographically pure, water is ultrapure water, and other reagents are analytically pure.
The schizandrol A reference substances have the batch numbers of 110857-contained 201211 and 110857-contained 201714, are purchased from China food and drug testing research institute and are used for content measurement.
2, liquid chromatography conditions and system applicability test:
yue Xue Welch Ultimate XB-C18 (4.6X 250mm X5 μm) chromatography column.
3, mobile phase: elution was carried out with a gradient [ acetonitrile (A) -water (B) as a mobile phase (0 min: 45% A → 25 min: 68% A → 40 min: 68% A → 60 min: 45% A) ]
Flow rate: 1.0mL/min
Detection wavelength: 250nm
Column temperature: 35 deg.C
Sample introduction volume: 10uL
The theoretical plate number is 5500 calculated according to the schizandrol A peak. The separation degree of the schizandrol A from the impurity peaks on the edges is 2.84 and is more than 1.5.
4 preparation of control solutions: precisely weighing appropriate amount of schizandrol A as reference substance, and adding methanol to obtain solution containing 0.15mg/mL of schizandrol A as reference substance solution.
5, preparation of test solution:
taking about 4g of the content of the product, precisely weighing, adding 5g of diatomite, uniformly mixing, then placing in a Soxhlet extractor, adding 50mL of methanol, heating and refluxing for 4 hours, recovering the solvent from the extracting solution, concentrating to dryness, adding methanol to dissolve residues, transferring to a 25mL measuring flask, adding methanol to the scale, shaking uniformly, filtering by using a 0.45-micrometer organic filter membrane, and taking the subsequent filtrate to obtain a sample solution.
6 blank test:
6.1 preparation of negative sample solution:
taking the negative sample lacking the schizandrol A, and preparing the negative sample solution according to the preparation method of the test sample solution.
6.2 blank test:
and (3) respectively injecting the schizandrol A reference substance solution, the traditional Chinese medicine capsule test substance solution and the negative sample solution into a high performance liquid chromatograph for determination, wherein the experimental result is as follows: no peak appears in the negative sample solution of the schisandra chinensis lacking medicinal material at the retention time corresponding to the control solution, which indicates that other medicinal materials in the formula do not interfere with the determination of the schizandrol A.
7 examination of the Linear relationship:
accurately weighing 12.79mg of schizandrol A reference substance, placing in a 25mL measuring flask, adding methanol to dissolve and dilute to scale, and shaking; precisely measuring reference substance solutions 1, 2, 3, 4 and 5mL, respectively placing in 10mL measuring bottles, adding methanol to dilute to scale, shaking uniformly to obtain schizandrol A reference substances with concentrations of 0.05116mg/mL, 0.10232mg/mL, 0.15348mg/mL, 0.20464mg/mL, 0.25580mg/mL and 0.5116mg/mL, sucking 10uL of the reference substance solution, injecting into a high performance liquid chromatograph, measuring peak area by the method, drawing a standard curve, and obtaining the result shown in the following table.
The result shows that the schizandrol A has good linear relation in the range of 0.51-5.12 ug, and the regression equation is that the linear equation is y ═ 22579x-209.1(r ═ 0.9991)
8 stability test
The test solution (00DJD01) was removed and the content of the sample was measured at 0 hour, 4 hours, 10 hours, 17 hours, and 24 hours after the preparation, respectively, according to the chromatographic conditions described above, and the results are shown in the following table.
The result shows that the RSD of the peak area of the schizandrol A in 0-24 hours is less than 2.0%, which indicates that the test solution is stable in 24 hours.
9 degree of precision experiment
According to the text method, the same sample (00DJD01) solution is repeatedly injected for 6 times under the chromatographic conditions, and the relative standard deviation RSD is less than 2.0 percent, and the result is shown in the following table.
The experimental result shows that the precision of the instrument is good.
10 reproducibility of the experiments
The results are shown in the following table, using 6 aliquots from sample (00DJD01) for 6 parallel extractions and measurements.
The results show that the relative standard deviation RSD of the schizandrol A is less than 2.0 percent, which indicates that the method has good reproducibility.
11 rate of recovery experiment
Precisely weighing 2.00g of the same batch of samples (00DJD01) with known content, and 9 parts (the content of the schizandrol A in the samples is 1.54mg/g according to the measurement result of finished products), adding a certain amount of schizandrol A reference substance into each sample, measuring the content according to a text method, and calculating the recovery rate, wherein the results are shown in the following table.
As a result: the average recovery rate of the sample is 100.2%, the relative standard deviation values are less than 2.0%, and the results show that the method has good recovery rate and is feasible.
Examination of 12 Range
Samples (00DJD01) were taken as indicated in 2.0g, 4.0g and 6.0g (50% lower concentration limit and 150% higher concentration limit) and tested as per the test solution preparation method, the results of which are given in the following table.
The result shows that the relative standard deviation RSD of the schizandrol A is less than 2.0 percent, which indicates that the method has good reproducibility.
13 durability
In the experiments, Welch Ultimate XB-C18 (4.6X 250 mm. times.5 μm), Watts RP18 (4.6X 250 mm. times.5 μm), YMC-Triart C18 (4.6X 250 mm. times.5 μm) were tested. The results show that the separation effect of the three chromatographic columns is good. The result shows that the experimental method has good reproducibility.
14 determination of sample content
The content of schisandrin A is measured by text method for three batches of samples, and two batches of samples are taken in parallel (see figures 4 and 5), and the results are shown in the following table.
According to the regulation of pharmacopoeia, the schisandra fruit contains schisandrin (C)24H32O7) Not less than 0.40%. The content of fructus Schisandrae in each g of capsule is calculated by astragaloside IV according to the proportion of fructus Schisandrae in the formula, and should not be less than 0.5 mg.
Claims (1)
1. A quality control method for a Chinese medicinal capsule with liver injury protecting effect comprises microscopic identification, thin layer identification and quantitative determination of effective components;
the traditional Chinese medicine capsule with the function of protecting liver injury is prepared by processing six medicinal materials of kudzuvine root, hovenia dulcis thunb, astragalus root, lucid ganoderma, schisandra fruit and galangal rhizome by a modern production process;
identifying the lucid ganoderma sporocarp in the traditional Chinese medicine capsule with the auxiliary protection function on liver injury by adopting a microscopic identification method, wherein the microscopic identification method comprises the following steps: taking the content of the capsule, grinding the content, screening the content by a No. 5 sieve, selecting a proper amount of powder, placing the powder on a cover glass, dropwise adding a chloral hydrate test solution, covering the cover glass, and observing the content under a microscope: the slender light brown hypha is scattered and distributed, is bent, has few branches and has the diameter of 3 to 7 microns;
qualitatively identifying radix astragali and its effective component astragaloside IV in the capsule by thin layer identification method, wherein the test solution, control solution and control solution are obtained by the following methods: grinding capsule content, collecting powder 12g, adding diethyl ether 60ml, shaking for 1 hr, filtering to remove filtrate, extracting the residue with methanol 60ml, heating under reflux for 1 hr, filtering, recovering solvent from the filtrate to dryness, dissolving the residue with water 30ml, extracting with water saturated n-butanol for 4 times (20 ml, 15ml, and 15 ml), mixing n-butanol solutions, washing with ammonia solution, recovering solvent from n-butanol solution to dryness, dissolving the residue with water 20ml, cooling, passing through a D101 type macroporous adsorption resin column, wherein the inner diameter of the D101 type macroporous adsorption resin column is 1.5cm, the height of the column is 15cm, eluting with 40ml of water, discarding the eluent, eluting with 50ml of 40% ethanol, discarding the eluent, eluting with 50ml of 70% ethanol, collecting the eluent, recovering the solvent until the solvent is dry, and dissolving the residue with 1ml of methanol to obtain a sample solution; preparing 3g of radix astragali, and preparing a reference medicinal solution by the same method; adding methanol into astragaloside IV reference substance to obtain 1mg solution per 1ml as reference substance solution; in the thin-layer identification process, absorbing 5-10 mu l of the test solution, the reference medicinal material solution and the reference solution, respectively dropping the solutions on the same silica gel G thin-layer plate, taking a lower layer solution of dichloromethane-methanol-water as a developing agent, wherein the ratio of dichloromethane to methanol to water is 12:8:3, developing, taking out, drying, spraying a 10% sulfuric acid ethanol solution, and heating at 105 ℃ until spots are clearly developed; in the thin-layer identification process, the chromatogram of the test sample and the chromatogram of the reference sample are in corresponding positions, and the same brown spots appear in sunlight; the ultraviolet lamp shows the same orange-yellow fluorescent spots under 365 nm;
The method for quantitatively measuring the effective component is to measure the effective component schisandrin by adopting a high performance liquid chromatography, wherein the preparation method of the test solution comprises the following steps: taking 4g of the content of the product, precisely weighing, adding 5g of diatomite, uniformly mixing, then placing in a Soxhlet extractor, adding 50mL of methanol, heating and refluxing for 4 hours, recovering a solvent from an extracting solution, concentrating to dryness, adding methanol to dissolve residues, transferring to a 25mL measuring flask, adding methanol to a scale, shaking up, filtering with a 0.45um organic filter membrane, and taking a subsequent filtrate to obtain a sample solution; the method for quantitatively measuring the functional components comprises the following steps of precisely sucking 10uL of each of a reference solution and a test solution, injecting the reference solution and the test solution into a liquid chromatograph, and measuring, wherein the chromatographic conditions are as follows: octadecylsilane chemically bonded silica is used as a filling agent; performing gradient elution by using acetonitrile A-water B as a mobile phase, wherein the gradient elution mode is 0 min: 45% A → 25 min: 68% A → 40 min: 68% A → 60 min: 45% A, and the detection wavelength is 250 nm; the theoretical plate number is not less than 3000 according to the peak value of schizandrol A; the content of the capsule per g contains fructus Schisandrae chinensis (calculated as schisandrin) not less than 0.5 mg.
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| CN102879516A (en) * | 2012-09-25 | 2013-01-16 | 南京中医药大学 | Method for identifying Buyang Huanwu soup and measuring content of Buyang Huanwu soup |
| CN103808842A (en) * | 2014-01-17 | 2014-05-21 | 黑龙江葵花药业股份有限公司 | Quality detection method for liver protection dropping pill of traditional Chinese medicine preparation |
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