CN112618630A - Compound thrombus-invigorating soft capsule and quality detection method thereof - Google Patents
Compound thrombus-invigorating soft capsule and quality detection method thereof Download PDFInfo
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Abstract
The invention relates to the technical field of traditional Chinese medicine pharmacy, in particular to a compound thrombus-invigorating soft capsule and a quality detection method thereof, and especially relates to a compound thrombus-invigorating soft capsule and a detection method of salvianolic acid B content in the compound thrombus-invigorating soft capsule. The compound thrombus-invigorating soft capsule comprises a capsule shell and contents, wherein the contents consist of effective dry paste powder, soybean oil, beeswax and polyethylene glycol; the effective dry extract powder comprises 800 portions of 600-containing notoginseng, 300 portions of 200-containing astragalus, 200 portions of 100-containing salvia miltiorrhiza and 300 portions of 200-containing figwort; the weight ratio of the effective dry paste powder to the soybean oil is 3-5: 5-7, and the addition ratio of the beeswax is 4-6wt% of the soybean oil. The method for detecting the content of the salvianolic acid B in the compound thrombus-invigorating capsule comprises the following steps: preparing a test solution, preparing a reference solution and measuring by adopting a high performance liquid chromatography.
Description
Technical Field
The invention relates to the technical field of biological extraction, in particular to a compound thrombus-invigorating capsule and a quality detection method thereof, and especially relates to a compound thrombus-invigorating soft capsule and a detection method of salvianolic acid B content in the compound thrombus-invigorating soft capsule.
Background
At present, cardiovascular and cerebrovascular diseases are common diseases seriously threatening the health of human beings, especially the middle-aged and old people over 50 years old. Because the cardiovascular and cerebrovascular diseases have the characteristics of acute onset and fierce coming, the common hard capsule and tablet dosage forms can not achieve the effect of quick onset, so the soft capsule is a main dosage form for treating the cardiovascular and cerebrovascular diseases because the soft capsule can achieve the effect of quick onset. The existing compound thrombus-invigorating capsule has serious adsorption of contents on a capsule shell, influences the uniformity of the contents and simultaneously influences the content detection to cause instability and large error. Salvianolic acid B is prepared by condensing three molecules of salvianic acid with one molecule of caffeic acid, is one of the most studied salvianolic acids, and has important pharmacological action on heart, brain, liver, kidney and other organs. The existing detection method for the content of salvianolic acid B in the compound thrombus-invigorating capsule has large error of the test result and large influence on the test result, and the determination is to be further improved.
Disclosure of Invention
In order to overcome the defects and shortcomings in the prior art, the invention aims to provide the compound thrombus-invigorating soft capsule, the content of the compound thrombus-invigorating soft capsule is not easily adsorbed by a capsule shell, the content is uniformly distributed, the content can be effectively detected, the detection precision is improved, the product quality is ensured, the product stability is good, and the compound thrombus-invigorating soft capsule has good curative effect on cardiovascular and cerebrovascular diseases.
The invention also aims to provide a detection method of the content of salvianolic acid B in the compound thrombus-invigorating capsule, which is used for detecting the quality of the compound thrombus-invigorating capsule, and the detection method can further effectively control the quality of the compound thrombus-invigorating capsule and realize the comprehensive evaluation of the preparation quality, thereby ensuring the stability of the product quality and the safety and effectiveness of clinical medication to the utmost extent; the detection method is scientific and reasonable, has controllable conditions, strong specificity and high stability, and has strong practicability.
The invention is realized by the following technical scheme: a compound thrombus-invigorating soft capsule comprises the following raw materials in parts by weight: comprises a capsule shell and contents, wherein the contents consist of effective dry paste powder, soybean oil, beeswax and polyethylene glycol; the effective dry paste powder comprises the following medicinal material extracts in parts by weight: 800 portions of 600-containing notoginseng, 300 portions of 200-containing astragalus root, 200 portions of 100-containing salvia miltiorrhiza and 300 portions of 200-containing figwort; the weight ratio of the effective dry paste powder to the soybean oil is 3-5: 5-7, and the addition ratio of the beeswax is 4-6wt% of the soybean oil; the capsule shell is prepared from 0.95-1.05 parts of gelatin, 0.3-0.5 part of glycerol and 0.8-1.2 parts of water by weight.
Furthermore, the adding proportion of the polyethylene glycol is 5-10 wt% of the soybean oil.
Further, the polyethylene glycol is polyethylene glycol 400.
Further, the effective dry paste powder comprises the following medicinal materials in parts by weight: 750 parts of pseudo-ginseng, 240 parts of astragalus, 150 parts of salvia miltiorrhiza and 240 parts of radix scrophulariae; the weight ratio of the effective dry paste powder to the soybean oil is 4: 6, the addition ratio of the beeswax is 5 wt% of the soybean oil, the addition ratio of the polyethylene glycol is 8 wt% of the soybean oil, and the capsule shell is prepared from 0.95-1.05 parts by weight of gelatin, 0.3-0.5 part by weight of glycerol and 0.8-1.2 parts by weight of water.
The invention also provides a quality detection method of the compound thrombus-invigorating capsule, namely a detection method of the content of salvianolic acid B in the compound thrombus-invigorating capsule, which comprises the following steps:
(1) preparation of a test solution: taking the compound thrombus-invigorating soft capsule, pouring out the content, adding an organic solvent for ultrasonic treatment, cooling, supplementing the weight loss by the organic solvent, shaking up and filtering to obtain a test solution;
(2) preparation of control solutions: weighing salvianolic acid B reference substance, and adding methanol solution to obtain reference substance solution;
(3) and (3) measuring by adopting a high performance liquid chromatography: using a high performance liquid chromatograph, and using octadecylsilane chemically bonded silica as a filling agent; performing gradient elution by taking acetonitrile-methanol-formic acid-water as a mobile phase; the wavelength of the ultraviolet light detector is 286 nm; and respectively sucking the reference solution and the test solution, injecting the reference solution and the test solution into a liquid chromatograph, measuring, and finally calculating the content of the salvianolic acid B in the test solution.
Further, in the step (1), the preparation of the test solution specifically comprises: taking a plurality of compound thrombus-invigorating soft capsules, pouring out contents of the soft capsules, uniformly mixing, taking 0.9-1.1g, weighing, putting into a conical flask with a plug, adding 25mL of 70% methanol, sealing the plug, weighing, carrying out ultrasonic treatment, cooling, weighing again, complementing the weight loss by 70% methanol, shaking up, and filtering to obtain a test solution.
Further, in the step (1), the power of the ultrasonic treatment is 280-320W, the frequency is 40-50KHz, and the treatment time is 50-70 min.
Further, in the step (1), the preparation of the reference solution specifically comprises: taking a proper amount of salvianolic acid B reference substance, precisely weighing, and adding 70% methanol to obtain a solution containing 0.1mg per 1mL to obtain a test solution.
Further, in the step (3), the high performance liquid chromatography is used for measuring, acetonitrile-methanol-formic acid-water is used as a mobile phase, and the weight ratio of the acetonitrile-methanol-formic acid-water is as follows: 9-11: 29-31: 0.8-1.2: 58-60 is mobile phase, and the flow rate is 0.9-1.1 mL/min.
Further, in the step (3), the high performance liquid chromatography is used for measuring, acetonitrile-methanol-formic acid-water is used as a mobile phase, and the weight ratio of the acetonitrile-methanol-formic acid-water is as follows: 10: 30: 1: 59 is the mobile phase, the flow rate is 1 mL/min.
The invention has the beneficial effects that: in the compound thrombus-invigorating soft capsule, the content is not easy to be adsorbed by the capsule shell, the content is uniformly distributed, the content of active substances in the content can be effectively detected, the detection precision is improved, the product quality is ensured, the product stability is good, and the curative effect on cardiovascular and cerebrovascular diseases is good.
The method for detecting the content of the salvianolic acid B in the compound thrombus-invigorating capsule can further effectively control the quality of the compound thrombus-invigorating capsule and realize the comprehensive evaluation of the preparation quality, thereby ensuring the stability of the product quality and the safety and the effectiveness of clinical medication to the maximum extent; the quality detection method has the advantages of stability, reliability, strong specificity, high accuracy and good reproducibility, can comprehensively and effectively control the quality of the compound thrombus-invigorating soft capsule, ensures the safety and effectiveness of clinical medication, and better meets the requirements of patients and markets.
Drawings
FIG. 1 is a diagram of a liquid chromatograph for the proprietary experiment in example 1;
FIG. 2 is a linear relationship chart of salvianolic acid B in example 1.
Detailed Description
For the understanding of those skilled in the art, the present invention will be further described with reference to the following examples and accompanying drawings 1-2, and the content of the embodiments is not intended to limit the present invention.
In a typical embodiment of the invention, the compound thrombus-invigorating soft capsule comprises the following raw materials in parts by weight: comprises a capsule shell and contents, wherein the contents consist of effective dry paste powder, soybean oil, beeswax and polyethylene glycol; the effective dry paste powder comprises the following medicinal material extracts in parts by weight: 800 portions of 600-containing notoginseng, 300 portions of 200-containing astragalus root, 200 portions of 100-containing salvia miltiorrhiza and 300 portions of 200-containing figwort; the weight ratio of the effective dry paste powder to the soybean oil is 3-5: 5-7, and the addition ratio of the beeswax is 4-6wt% of the soybean oil; the capsule shell is prepared from 0.95-1.05 parts of gelatin, 0.3-0.5 part of glycerol and 0.8-1.2 parts of water by weight.
Furthermore, the adding proportion of the polyethylene glycol is 5-10 wt% of the soybean oil.
Further, the polyethylene glycol is polyethylene glycol 400.
Further, the effective dry paste powder comprises the following medicinal materials in parts by weight: 750 parts of pseudo-ginseng, 240 parts of astragalus, 150 parts of salvia miltiorrhiza and 240 parts of radix scrophulariae; the weight ratio of the effective dry paste powder to the soybean oil is 4: 6, the addition ratio of the beeswax is 5 wt% of the soybean oil, the addition ratio of the polyethylene glycol is 8 wt% of the soybean oil, and the capsule shell is prepared from 0.95-1.05 parts by weight of gelatin, 0.3-0.5 part by weight of glycerol and 0.8-1.2 parts by weight of water.
The preparation method of the compound thrombus-invigorating capsule refers to patent application 201410847417.1 'A compound thrombus-invigorating soft capsule and a preparation process thereof' proposed by the applicant in 2014, except that in the preparation step of the capsule content, the invention is to uniformly mix pseudo-ginseng dry paste powder and the rest medicinal material dry paste powder, and then add beeswax, soybean oil and polyethylene glycol 400 according to the weight ratio, and the patent application document does not add polyethylene glycol 400.
The invention also provides a method for detecting the content of salvianolic acid B in the compound thrombus-invigorating capsule, which comprises the following steps:
(1) preparation of a test solution: taking the compound thrombus-invigorating soft capsule, pouring out the content, adding an organic solvent for ultrasonic treatment, cooling, supplementing the weight loss by the organic solvent, shaking up and filtering to obtain a test solution;
(2) preparation of control solutions: weighing salvianolic acid B reference substance, and adding methanol solution to obtain reference substance solution;
(3) and (3) measuring by adopting a high performance liquid chromatography: using a high performance liquid chromatograph, and using octadecylsilane chemically bonded silica as a filling agent; performing gradient elution by taking acetonitrile-methanol-formic acid-water as a mobile phase; the wavelength of the ultraviolet light detector is 286 nm; and respectively sucking the reference solution and the test solution, injecting the reference solution and the test solution into a liquid chromatograph, measuring, and finally calculating the content of the salvianolic acid B in the test solution.
Further, in the step (1), the preparation of the test solution specifically comprises: taking a plurality of compound thrombus-invigorating soft capsules, pouring out contents of the soft capsules, uniformly mixing, taking 0.9-1.1g, weighing, putting into a conical flask with a plug, adding 25mL of 70% methanol, sealing the plug, weighing, carrying out ultrasonic treatment, cooling, weighing again, complementing the weight loss by 70% methanol, shaking up, and filtering to obtain a test solution.
Further, in the step (1), the power of the ultrasonic treatment is 280-320W, the frequency is 40-50KHz, and the treatment time is 50-70 min.
Further, in the step (1), the preparation of the reference solution specifically comprises: taking a proper amount of salvianolic acid B reference substance, precisely weighing, and adding 70% methanol to obtain a solution containing 0.1mg per 1mL to obtain a test solution.
Further, in the step (3), the high performance liquid chromatography is used for measuring, acetonitrile-methanol-formic acid-water is used as a mobile phase, and the weight ratio of the acetonitrile-methanol-formic acid-water is as follows: 9-11: 29-31: 0.8-1.2: 58-60 is mobile phase, and the flow rate is 0.9-1.1 mL/min.
Example 1
In the embodiment, the compound thrombus-invigorating soft capsule comprises the following raw materials in parts by weight: comprises a capsule shell and contents, wherein the contents consist of effective dry paste powder, soybean oil, beeswax and polyethylene glycol; the effective dry paste powder comprises the following medicinal material extracts in parts by weight: 750 parts of pseudo-ginseng, 240 parts of astragalus, 150 parts of salvia miltiorrhiza and 240 parts of radix scrophulariae; the weight ratio of the effective dry paste powder to the soybean oil is 4: 6, and the addition ratio of the beeswax is 5 wt% of the soybean oil; the capsule shell is prepared from 1 part of gelatin, 0.4 part of glycerin and 1 part of water in parts by weight. The prepared compound thrombus-invigorating soft capsule has the specification of 0.74 g.
Furthermore, the adding proportion of the polyethylene glycol is 5-10 wt% of the soybean oil.
Further, the polyethylene glycol is polyethylene glycol 400.
1 test Material
1.1 Instrument: saimeifei U3000 liquidA phase chromatograph (composed of an LPG-3400SDN infusion pump, a WPS-3000SL automatic sample injector, a TCC-3000SD column incubator and a VWD-3400RS ultraviolet detector); an electronic balance: sartorius BP211D, SQP; an ultrasonic instrument: AS10200AD ultrasonic cleaner; a chromatographic column: syncronis C18(250 mm. times.4.6 mm, 5 μm); yueuxu XB-C18(250 mm. times.4.6 mm, 5 μm); agilent 5TC-C18(2) (250 mm. times.4.6 mm, 5 μm).
1.2 reagent: acetonitrile is chromatographically pure, methanol is chromatographically pure and analytically pure, water is ultrapure water, and formic acid is analytically pure.
1.3 comparison products: salvianolic acid B (94.1% in terms of content) was purchased from the institute of food and drug testing, China.
1.4 test article: the compound thrombus-invigorating capsule and the salvia miltiorrhiza negative sample prepared in the example are both produced by Guangdong Guangfu pharmaceutical Co.
Further, the effective dry paste powder comprises the following medicinal materials in parts by weight: 750 parts of pseudo-ginseng, 240 parts of astragalus, 150 parts of salvia miltiorrhiza and 240 parts of radix scrophulariae; the weight ratio of the effective dry paste powder to the soybean oil is 4: 6, the addition ratio of the beeswax is 5 wt% of the soybean oil, the addition ratio of the polyethylene glycol is 8 wt% of the soybean oil, and the capsule shell is prepared from 0.95-1.05 parts by weight of gelatin, 0.3-0.5 part by weight of glycerol and 0.8-1.2 parts by weight of water.
2 record of the test
2.1 chromatographic conditions using octadecylsilane chemically bonded silica as filler; acetonitrile-methanol-formic acid-water (10: 30: 1: 59) as a mobile phase; the flow rate is 1 ml/min; the wavelength of the ultraviolet light detector is as follows: 286 nm. The number of theoretical plates is not less than 2000 calculated according to salvianolic acid B peak.
2.2 preparation of control solution an appropriate amount of salvianolic acid B control was precisely weighed and added with 70% methanol to make a solution containing 0.1mg per 1 ml.
2.3 preparing test solution by taking 10 compound thrombus-invigorating soft capsules, pouring out the content, mixing uniformly, taking 1.0g, precisely weighing, placing in a conical flask with a plug, precisely adding 25ml of 70% methanol, sealing the plug, weighing, ultrasonically treating (power 300W, frequency 45KHz) for 60 minutes, cooling, weighing again, supplementing the lost weight with 70% methanol, shaking uniformly, and filtering to obtain the compound thrombus-invigorating capsule.
2.4 measuring, respectively and precisely sucking 10 μ l of reference solution and sample solution, injecting into liquid chromatograph, and measuring.
3 methodological validation
3.1 accuracy test about 0.5g of the same batch of samples (batch No. 20191001, each containing 1.87mg of salvianolic acid B) with known content was precisely weighed, 9 parts were precisely weighed, 25ml of salvianolic acid B control solution (low concentration 22.7. mu.g/ml, medium concentration 45.3. mu.g/ml, high concentration 79.9. mu.g/ml) was precisely added, and a recovered sample solution was prepared according to the method for preparing a sample solution under "2.3". The recovery rate of salvianolic acid B is calculated according to the chromatographic condition measurement under the item of 2.1. As a result: the average recovery rate of salvianolic acid B was 101.3% and RSD was 2.0% (n ═ 9). The accuracy of the method is better (see table 1).
TABLE 1 Salvianolic acid B accuracy (sample recovery) test results
3.2 repeatability test Compound XUESHUANTONG Soft Capsule is taken, about 1g, 6 parts in total, precisely weighed, prepared into test solution according to the method under item "2.3", and measured according to the chromatographic conditions under item "2.1", with the results shown in Table 2. The average content of salvianolic acid B was 1.87 mg/capsule and RSD was 1.3% (n ═ 6).
TABLE 2 results of the repeatability tests
3.3 the special test sucks 10 mul of reference solution, test solution and negative sample solution respectively, and injects them into a liquid chromatograph, the result shows that the negative sample without interference, the result is shown in figure 1.
3.4 investigation of Linear relationship Salvianolic acid B (lot No. 111562-201716)10mg was precisely weighed, placed in a 10ml volumetric flask, dissolved by adding a proper amount of methanol, added to a proper amount of scale, shaken up to obtain a stock solution of a reference solution, and the stock solution was diluted with 70% methanol to obtain a reference solution of a corresponding concentration. The control solutions with corresponding volumes were respectively extracted and injected into a liquid chromatograph, and the peak areas were measured under the chromatographic conditions of "2.1", and the results are shown in table 3.
TABLE 3 examination of the Linear relationship
Taking the sample amount (μ g) (X) as the abscissa and the peak area (Y) as the ordinate, the linear regression equation is: danshinolic acid B y ═ 21.821x +0.493, R20.9997. The results show that: the linear relation of the salvianolic acid B is in the range of 0.1699-2.2660 ng, and the result is shown in figure 2.
3.5 investigation of durability
The influence of wavelength, chromatographic column, flow rate, column temperature, extraction solvent and ultrasonic time on the measurement is respectively inspected, and the result shows that (see table 4) different flow rates, column temperatures, chromatographic columns, wavelengths and the like are adopted, the RSD of the content measurement result of each component is less than or equal to 2.0 percent, and the method has good durability.
Table 4 results of content measurement of each component using different flow rates, column temperatures, chromatography columns, wavelengths, etc
3.6 investigation of sample solution stability
For the sample solution (under the precision term), 10ul of the sample solution is absorbed at 0h, 4h, 9h, 12h and 24h and injected into a liquid chromatograph, and the results are shown in table 5, which shows that the differences between the detection results and the initial values of the sample solution after being placed at room temperature for 4h, 9h, 12h and 24h are all less than or equal to 2.0%.
Table 5 sample solution stability verification record results
| Serial number | Time | Peak area of salvianolic acid B | Relative deviation from |
| 1 | 0h | 20.322 | / |
| 2 | 4h | 20.274 | 0.2％ |
| 3 | 9h | 20.293 | 0.1％ |
| 4 | 12h | 20.307 | 0.1％ |
| 5 | 24h | 20.326 | 0.1％ |
3.7 results of sample testing of example 1 (see Table 6)
TABLE 66 measurement of the contents of the samples in batches
Example 2
A compound thrombus-invigorating soft capsule comprises the following raw materials in parts by weight: comprises a capsule shell and contents, wherein the contents consist of effective dry paste powder, soybean oil, beeswax and polyethylene glycol; the effective dry paste powder comprises the following medicinal material extracts in parts by weight: 600 parts of pseudo-ginseng, 200 parts of astragalus, 100 parts of salvia miltiorrhiza and 200 parts of radix scrophulariae; the weight ratio of the effective dry paste powder to the soybean oil is 3: 5, and the addition ratio of the beeswax is 4 wt% of the soybean oil; the capsule shell is prepared from 0.95 part of gelatin, 0.3 part of glycerol and 0.8 part of water in parts by weight.
Further, the addition ratio of the polyethylene glycol is 5 wt% of the soybean oil.
The rest of this embodiment is the same as embodiment 1, and is not described herein again.
Example 3
A compound thrombus-invigorating soft capsule comprises the following raw materials in parts by weight: comprises a capsule shell and contents, wherein the contents consist of effective dry paste powder, soybean oil, beeswax and polyethylene glycol; the effective dry paste powder comprises the following medicinal material extracts in parts by weight: 800 parts of pseudo-ginseng, 300 parts of astragalus, 200 parts of salvia miltiorrhiza and 300 parts of radix scrophulariae; the weight ratio of the effective dry paste powder to the soybean oil is 5: 7, and the addition ratio of the beeswax is 6wt% of the soybean oil; the capsule shell is prepared from 1.05 parts of gelatin, 0.5 part of glycerol and 1.2 parts of water by weight.
Further, the addition ratio of the polyethylene glycol is 10 wt% of the soybean oil.
The rest of this embodiment is the same as embodiment 1, and is not described herein again.
Example 4
A compound thrombus-invigorating soft capsule comprises the following raw materials in parts by weight: comprises a capsule shell and contents, wherein the contents consist of effective dry paste powder, soybean oil, beeswax and polyethylene glycol; the effective dry paste powder comprises the following medicinal material extracts in parts by weight: 650 parts of pseudo-ginseng, 240 parts of astragalus, 140 parts of salvia miltiorrhiza and 250 parts of radix scrophulariae; the weight ratio of the effective dry paste powder to the soybean oil is 3.5: 5.5, and the addition ratio of the beeswax is 4.5 wt% of the soybean oil; the capsule shell is prepared from 1 part of gelatin, 0.4 part of glycerin and 1 part of water in parts by weight.
The rest of this embodiment is the same as embodiment 1, and is not described herein again.
The above-described embodiments are preferred implementations of the present invention, and the present invention may be implemented in other ways without departing from the spirit of the present invention.
Claims (10)
1. A compound thrombus-invigorating soft capsule is characterized in that: the feed comprises the following raw materials in parts by weight: comprises a capsule shell and contents, wherein the contents consist of effective dry paste powder, soybean oil, beeswax and polyethylene glycol; the effective dry paste powder comprises the following medicinal material extracts in parts by weight: 800 portions of 600-containing notoginseng, 300 portions of 200-containing astragalus root, 200 portions of 100-containing salvia miltiorrhiza and 300 portions of 200-containing figwort; the weight ratio of the effective dry paste powder to the soybean oil is 3-5: 5-7, and the addition ratio of the beeswax is 4-6wt% of the soybean oil; the capsule shell is prepared from 0.95-1.05 parts of gelatin, 0.3-0.5 part of glycerol and 0.8-1.2 parts of water by weight.
2. The compound thrombus-invigorating soft capsule according to claim 1, which is characterized in that: the addition proportion of the polyethylene glycol is 5-10 wt% of the soybean oil.
3. The compound thrombus-invigorating soft capsule according to claim 1, which is characterized in that: the polyethylene glycol is polyethylene glycol 400.
4. The compound thrombus-invigorating soft capsule according to claim 1, which is characterized in that: the effective dry paste powder comprises the following medicinal materials in parts by weight: 750 parts of pseudo-ginseng, 240 parts of astragalus, 150 parts of salvia miltiorrhiza and 240 parts of radix scrophulariae; the weight ratio of the effective dry paste powder to the soybean oil is 4: 6, the addition ratio of the beeswax is 5 wt% of the soybean oil, the addition ratio of the polyethylene glycol is 8 wt% of the soybean oil, and the capsule shell is prepared from 0.95-1.05 parts by weight of gelatin, 0.3-0.5 part by weight of glycerol and 0.8-1.2 parts by weight of water.
5. A method for detecting the content of salvianolic acid B in the compound thrombus-invigorating capsule as claimed in any one of claims 1 to 4, which is characterized in that: the method comprises the following steps:
(1) preparation of a test solution: taking the compound thrombus-invigorating soft capsule, pouring out the content, adding an organic solvent for ultrasonic treatment, cooling, supplementing the weight loss by the organic solvent, shaking up and filtering to obtain a test solution;
(2) preparation of control solutions: weighing salvianolic acid B reference substance, and adding methanol solution to obtain reference substance solution;
(3) and (3) measuring by adopting a high performance liquid chromatography: using a high performance liquid chromatograph, and using octadecylsilane chemically bonded silica as a filling agent; performing gradient elution by taking acetonitrile-methanol-formic acid-water as a mobile phase; the wavelength of the ultraviolet light detector is 286 nm; and respectively sucking the reference solution and the test solution, injecting the reference solution and the test solution into a liquid chromatograph, measuring, and finally calculating the content of the salvianolic acid B in the test solution.
6. The method for detecting the content of salvianolic acid B in the compound thrombus-invigorating capsule as claimed in claim 1, which is characterized in that: in the step (1), the preparation of the test solution specifically comprises the following steps: taking a plurality of compound thrombus-invigorating soft capsules, pouring out contents of the soft capsules, uniformly mixing, taking 0.9-1.1g, weighing, putting into a conical flask with a plug, adding 25mL of 70% methanol, sealing the plug, weighing, carrying out ultrasonic treatment, cooling, weighing again, complementing the weight loss by 70% methanol, shaking up, and filtering to obtain a test solution.
7. The method for detecting the content of salvianolic acid B in the compound thrombus-invigorating capsule as claimed in claim 6, which is characterized in that: in the step (1), the power of ultrasonic treatment is 280-320W, the frequency is 40-50KHz, and the treatment time is 50-70 min.
8. The method for detecting the content of salvianolic acid B in the compound thrombus-invigorating capsule as claimed in claim 1, which is characterized in that: in the step (1), the preparation of the reference solution specifically comprises the following steps: taking a proper amount of salvianolic acid B reference substance, precisely weighing, and adding 70% methanol to obtain a solution containing 0.1mg per 1mL to obtain a test solution.
9. The method for detecting the content of salvianolic acid B in the compound thrombus-invigorating capsule as claimed in claim 1, which is characterized in that: in the step (3), acetonitrile-methanol-formic acid-water is used as a mobile phase for determination by high performance liquid chromatography, and the weight ratio of the acetonitrile-methanol-formic acid-water is as follows: 9-11: 29-31: 0.8-1.2: 58-60 is mobile phase, and the flow rate is 0.9-1.1 mL/min.
10. The method for detecting the content of salvianolic acid B in the compound thrombus-invigorating capsule as claimed in claim 1, which is characterized in that: in the step (3), acetonitrile-methanol-formic acid-water is used as a mobile phase for determination by high performance liquid chromatography, and the weight ratio of the acetonitrile-methanol-formic acid-water is as follows: 10: 30: 1: 59 is the mobile phase, the flow rate is 1 mL/min.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114848744A (en) * | 2022-04-26 | 2022-08-05 | 杭州市中医院 | Traditional Chinese medicine composition for treating qi deficiency and blood stasis type coronary heart disease and preparation method thereof |
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| CN114848744A (en) * | 2022-04-26 | 2022-08-05 | 杭州市中医院 | Traditional Chinese medicine composition for treating qi deficiency and blood stasis type coronary heart disease and preparation method thereof |
| CN114848744B (en) * | 2022-04-26 | 2023-08-15 | 杭州市中医院 | Traditional Chinese medicine composition for treating qi deficiency and blood stasis type coronary heart disease and preparation method thereof |
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