Quality detection method and application of ginkgo ginseng preparation

Abstract

The application provides a quality detection method and application of ginkgo ginseng preparation, and relates to the technical field of pharmaceutical analysis. The quality detection method comprises the following steps: crushing and sieving the ginkgo ginseng preparation, weighing, adding a solvent for extraction, filtering with a filter membrane, evaporating the filtrate, dissolving the residue with methanol, constant volume, and obtaining a test sample solution; the solvent is a mixed solution of n-butanol, methanol and ethyl acetate; a control sample of ginkgo lactone, ginkgo lactone A, ginkgo lactone B, ginkgo lactone C, ginsenoside F11, ginsenoside Rb1, ginsenoside Re and ginsenoside Rg1 is weighed, mixed with a solvent, and a control sample solution is obtained; a liquid chromatograph is used to determine the control sample solution and the test sample solution, and a chromatogram is obtained; the quality detection method has the advantages of simplicity, rapidness, stability, reliability, high precision, good reproducibility, easy operation and the like, and can simultaneously detect the above-mentioned saponins and lactones and the like.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of pharmaceutical analysis, in particular to a quality detection method and application of ginkgo and American ginseng preparation. BACKGROUND

[0002] The main raw material of ginkgo and American ginseng preparation is ginkgo leaf and American ginseng, which has the effect of benefiting qi and activating blood, and widening chest and unblocking vessels. It is used for the auxiliary treatment of qi deficiency and blood stasis syndrome of coronary heart disease (chest pain), and has improvement effect on symptoms such as chest tightness, shortness of breath and palpitation.

[0003] American ginseng (Panax quinquefolium L.) contains saponins, nucleotides, active polysaccharides, proteins, amino acids, inorganic elements and flavonoids, and has many pharmacological effects such as immunomodulation, anti-depression, anti-tumor, anti-inflammatory, anti-oxidation and blood lipid lowering. The quality of American ginseng is good or bad, which brings hidden dangers to the safe use of clinical medicine. The quality of raw medicine greatly determines the quality of its preparation and health food, and the quality detection and control of raw medicine is of great significance to ensure the clinical efficacy.

[0004] Ginkgo leaf is the dried leaf of Ginkgo biloba Linn. of Ginkgoaceae, which is mainly used for treating cardiovascular and cerebrovascular diseases and nervous system diseases. Terpenelactones and flavonoids contained in ginkgo leaf are the main medicinal active ingredients of ginkgo leaf.

[0005] Chinese patent CN102309531B discloses a method for determining the fingerprint spectrum of American ginseng medicinal material. The method determines the fingerprint spectrum by high performance liquid chromatography, and detects by evaporative light scattering detector. The chromatographic conditions of the high performance liquid chromatography are as follows: the chromatographic column is C18 column; the mobile phase: mobile phase A is acetonitrile, and mobile phase B is 0.05% acetic acid aqueous solution, gradient elution,

[0006] The gradient of the mobile phase is as follows:

[0007] 0→20 minutes, mobile phase A is uniformly reduced from 80% to 79%, 20→25 minutes, mobile phase A is uniformly reduced from 79% to 74%, 25→29 minutes, mobile phase A is uniformly reduced from 74% to 73%, 29→43 minutes, mobile phase A is uniformly reduced from 73% to 66%, 43→47 minutes, mobile phase A is uniformly reduced from 66% to 64%, 47→54 minutes, mobile phase A is uniformly reduced from 64% to 57%, 54→55 minutes, mobile phase A is uniformly reduced from 57% to 55%, 55→59 minutes, mobile phase A is uniformly reduced from 55% to 50%, 59→65 minutes, mobile phase A is uniformly reduced from 50% to 5%, 65→69 minutes, mobile phase A is kept at 5%. However, this scheme only controls the quality of active ingredients of American ginseng.

[0008] The Chinese patent CN 115112783 A provides a ginkgo leaf fingerprint detection method, which comprises the following steps: taking ginkgo leaf reference substance and test sample for detection, and the chromatographic conditions of the detection comprise: the chromatographic column is ZORBAX SB-C18 (4.6*250 mm, 5 μm); the mobile phase is 0.1 volume % formic acid water (A)-methanol (B); the gradient elution program is: 0-10 min: 90 volume %-80 volume % A; 10-25 min: 80 volume %-70 volume % A; 25-35 min: 70 volume % A; 35-45 min: 70 volume %-58 volume % A; 45-70 min: 58 volume %-45 volume % A; 70-85 min: 45 volume %-30 volume % A; 85-95 min: 30 volume %-5 volume % A; 95-115 min: 5 volume % A. The flow rate is 0.9-1.1 mL / min; the detection wavelength is 360 nm, the column temperature is 25-35 DEG C, the injection amount is 10 μL; the evaporation light scattering detector parameters: the drift tube temperature is 110 DEG C, the carrier gas flow rate is 3.0 mL / min, and the gain value is 4. A reliable analysis method is provided for effective control of the quality of ginkgo leaf preparations. However, the scheme is only for the quality control of active ingredients of ginkgo leaves.

[0009] Traditional Chinese medicine fingerprint has the characteristics of whole, macro, fuzzy analysis, etc. Through the description of the whole characteristics of traditional Chinese medicine, appropriate fuzzy processing method is adopted to achieve the purpose of whole quality control, so it becomes an effective means of traditional Chinese medicine quality control. The chromatographic fingerprint analysis can make the whole characteristics of various chemical components in traditional Chinese medicine visualized, so as to expose the quality problems that cannot be found by conventional inspection. However, there is no quality control method for the active ingredients of ginkgo ginseng preparation at present. SUMMARY

[0010] The present application provides a quality detection method for ginkgo ginseng preparation, which can realize the separation and detection of active ingredients in ginkgo ginseng preparation by optimizing the pretreatment method of the sample, the elution solvent and the elution program, and can make a more comprehensive and accurate evaluation on the quality of ginkgo ginseng preparation.

[0011] In order to achieve the above-mentioned purpose, the technical scheme adopted by the present application is as follows:

[0012] On the one hand, the present application provides a quality detection method for ginkgo ginseng preparation, which comprises the following steps:

[0013] S1: preparation of test sample solution: taking ginkgo ginseng preparation, crushing, sieving, weighing, adding solvent for extraction, filtering membrane filtration, evaporating the filtrate to dryness, dissolving the residue with methanol, and constant volume to obtain the test sample solution; the solvent is a mixed solution of n-butanol, methanol and ethyl acetate;

[0014] S2: Preparation of the control solution: the control substance ginkgolide, ginkgolide A, ginkgolide B, ginkgolide C, ginsenoside F11, ginsenoside Rb1, ginsenoside Re and ginsenoside Rg1 are weighed and mixed with the solvent to obtain the control solution;

[0015] S3: The control solution and the test solution are determined by using a liquid chromatograph to obtain a chromatogram;

[0016] The chromatographic conditions are as follows:

[0017] Chromatographic column: non-polar reverse phase chromatographic column;

[0018] Mobile phase:

[0019] Mobile phase A: acetonitrile and chloroform;

[0020] Mobile phase B: 0.15-0.3wt% phosphoric acid solution and 0.01-0.015wt% acetic acid solution;

[0021] Flow rate: 0.8-1.2mL·min -1 ;

[0022] Column temperature: 30-40℃;

[0023] The elution mode is gradient elution, and the elution gradient is as follows:

[0024] 0-5min, volume ratio of mobile phase A to mobile phase B: 8-10:90-92;

[0025] 5-15min, volume ratio of mobile phase A to mobile phase B: 8-18:82-92;

[0026] 15-20min, volume ratio of mobile phase A to mobile phase B: 10-28:72-90;

[0027] 20-50min, volume ratio of mobile phase A to mobile phase B: 23-35:65-77;

[0028] 50-70min, volume ratio of mobile phase A to mobile phase B: 25-80:20-75.

[0029] Preferably, in S1, the sieving is sieving through a 40-60 mesh sieve; further preferably, in S1, the sieving is sieving through a 40 mesh sieve.

[0030] Preferably, in S1, the ratio of the ginkgo and ginseng preparation to the solvent is 1:10-20g / mL; further preferably, in S1, the ratio of the ginkgo and ginseng preparation to the solvent is 1:14g / mL.

[0031] Preferably, in S1, the extraction is ultrasonic extraction;

[0032] Preferably, the parameters of the ultrasonic extraction are: the power of the ultrasonic is 300-550 W, the frequency is 30-40 kHz, and the time is 20-45 min; further preferably, the parameters of the ultrasonic extraction are: the power of the ultrasonic is 420 W, the frequency is 35 kHz, and the time is 35 min.

[0033] Preferably, in S1, the pore size of the filter membrane is 0.2-0.35 μm, and further preferably, in S1, the pore size of the filter membrane is 0.24 μm.

[0034] Preferably, in S1, the concentration of the test sample solution is 1 g / 50 mL.

[0035] Preferably, in S1, in the mixed solution of n-butanol, methanol and ethyl acetate, the methanol is a methanol solution with a volume fraction of 70-85%; further preferably, in S1, in the mixed solution of n-butanol, methanol and ethyl acetate, the methanol is a methanol solution with a volume fraction of 85%.

[0036] Preferably, in S1, the volume ratio of n-butanol, methanol and ethyl acetate is 8-12:5-7.5:0.5-1.5; further preferably, in S1, the volume ratio of n-butanol, methanol and ethyl acetate is 10:6.5:1.

[0037] Preferably, in S2, the concentration of each control in the control solution is: 10-14 μg / mL of ginkgolide, 6-14 μg / mL of ginkgo biloba extract A, 5-12 μg / mL of ginkgo biloba extract B, 1-16 μg / mL of ginkgo biloba extract C, 7-15 μg / mL of ginsenoside F11, 80-130 μg / mL of ginsenoside Rb1, 50-80 μg / mL of ginsenoside Re, and 1-10 μg / mL of ginsenoside Rg1; further preferably, in S2, the concentration of each control in the control solution is: 12 μg / mL of ginkgolide, 8 μg / mL of ginkgo biloba extract A, 7 μg / mL of ginkgo biloba extract B, 6 μg / mL of ginkgo biloba extract C, 12 μg / mL of ginsenoside F11, 120 μg / mL of ginsenoside Rb1, 60 μg / mL of ginsenoside Re, and 5 μg / mL of ginsenoside Rg1.

[0038] Preferably, in S2, the solvent is a mixture of a methanol solution with a volume fraction of 85% and acetonitrile;

[0039] Preferably, the volume ratio of the methanol solution with a volume fraction of 85% and acetonitrile is 8-12:1; further preferably, the volume ratio of the methanol solution with a volume fraction of 85% and acetonitrile is 10:1.

[0040] Preferably, in S3, the chromatographic column is a non-polar reverse phase chromatographic column with octadecylsilane-bonded silica gel as the filler.

[0041] Preferably, in S3, the volume ratio of acetonitrile and chloroform in the mobile phase A is 8-12:1; further preferably, in S3, the volume ratio of acetonitrile and chloroform in the mobile phase A is 9:1.

[0042] Preferably, in S3, the mobile phase B is a 0.25wt% phosphoric acid solution and a 0.01wt% acetic acid solution.

[0043] Preferably, in S3, the volume ratio of the 0.25wt% phosphoric acid solution and the 0.01wt% acetic acid solution in the mobile phase B is 3-5:1; further preferably, in S3, the volume ratio of the 0.25wt% phosphoric acid solution and the 0.01wt% acetic acid solution in the mobile phase B is 4:1.

[0044] Preferably, in S3, the flow rate is 1mL·min -1 ;

[0045] Preferably, in S3, the column temperature is 35℃.

[0046] Preferably, in S3, the detection wavelength of the chromatographic conditions is 280-310nm.

[0047] Preferably, in S3, the elution gradient is:

[0048] Time / min Mobile phase A / Vt% Mobile phase B / Vt% 0 10 90 5 10 90 15 14 86 20 25 75 35 30 70 50 30 70 60 78 22 70 78 22

[0049] In another aspect, the application provides the use of the quality detection method of the above-mentioned ginkgo and American ginseng preparation in the quality control of ginkgo and American ginseng preparations using ginkgo leaves and American ginseng as raw materials.

[0050] Preferably, the ginkgo and American ginseng preparation comprises ginkgo and American ginseng capsules and ginkgo and American ginseng granules.

[0051] Compared with the prior art, the application has the following beneficial effects:

[0052] 1. The technical scheme of the application ensures that each effective component in the ginkgo and American ginseng preparation is extracted to the maximum extent, and comprehensive effective component information is obtained, by optimizing the extraction solvent and extraction time.

[0053] 2. The quality determination method of the ginkgo ginseng preparation provided by the application can overcome the interference caused by the complex chemical components of traditional Chinese medicines under the preferred chromatographic conditions, so that the quality of the ginkgo ginseng preparation can be comprehensively and clearly detected.

[0054] 3. The quality detection method has the advantages of simplicity, rapidness, stability, reliability, high precision, good reproducibility and easy mastery. DETAILED DESCRIPTION

[0055] In order to make the technical means, creative features, purposes and effects realized by the application easy to understand, the application will be further illustrated below in combination with specific embodiments, but the following embodiments are only preferred embodiments of the application, not all. Based on the embodiments in the embodiments, other embodiments obtained by those skilled in the art without creative labor all belong to the protection scope of the application. It is worth noting that the raw materials used in the application are all ordinary commercially available products, and their sources are not specifically limited. The technologies and scientific terms used in the embodiments have the meanings commonly understood by those skilled in the art to which the application belongs.

[0056] Instruments and reagents

[0057] Agilent 1260Infinity II liquid chromatograph (vacuum degassing machine, binary pump, automatic sampler, column oven, DAD detector);

[0058] Analytical balance, model: Mettler Toledo PL203 and XS205;

[0059] KQ-300DB type numerical control ultrasonic cleaner (300W, 40kHz).

[0060] Phosphoric acid, manufacturer: National Pharmaceutical Group Chemical Reagent Co., Ltd.;

[0061] Acetic acid, manufacturer: National Pharmaceutical Group Chemical Reagent Co., Ltd.;

[0062] Methanol, manufacturer: National Pharmaceutical Group Chemical Reagent Co., Ltd.;

[0063] Acetonitrile, manufacturer: National Pharmaceutical Group Chemical Reagent Co., Ltd.;

[0064] n-Butanol, manufacturer: National Pharmaceutical Group Chemical Reagent Co., Ltd.;

[0065] Ethyl acetate, manufacturer: National Pharmaceutical Group Chemical Reagent Co., Ltd.;

[0066] Water, purified water.

[0067] Sample: Ginkgo ginseng preparation (produced by Guangxi Liangmianjian Yikang Pharmaceutical Co., Ltd.).

[0068] Reference substances: ginkgolide, ginkgolide A, ginkgolide B, ginkgolide C, ginsenoside F11, ginsenoside Rb1, ginsenoside Re and ginsenoside Rg1 were purchased from China Institute for Food and Drug Control, and other reagents were required to be of analytical purity.

[0069] Example 1

[0070] A quality detection method of ginkgo and ginseng preparation, specifically:

[0071] S1: Preparation of test sample solution: ginkgo and ginseng preparation was taken, crushed, passed through a 40-mesh sieve, weighed, extracted with a solvent, the solid-liquid ratio of ginkgo and ginseng preparation to solvent was 1:14 g / mL, filtered through a 0.24-μm filter membrane, the filtrate was evaporated to dryness, the residue was dissolved in methanol, and the volume was made up to obtain the test sample solution; the concentration of the test sample solution was 1 g / 50 mL;

[0072] The solvent was a mixed solution of n-butanol, 85% (by volume) methanol and ethyl acetate; the volume ratio of n-butanol, 85% (by volume) methanol and ethyl acetate was 10:6.5:1.

[0073] S2: Preparation of reference substance solution: reference substances ginkgolide, ginkgolide A, ginkgolide B, ginkgolide C, ginsenoside F11, ginsenoside Rb1, ginsenoside Re and ginsenoside Rg1 were weighed, mixed with a solvent to obtain the reference substance solution; the solvent was a mixture of 85% (by volume) methanol solution and acetonitrile; the volume ratio of 85% (by volume) methanol solution and acetonitrile was 10:1.

[0074] The concentration of each reference substance in the reference substance solution was: ginkgolide 8 μg / mL, ginkgolide A 12 μg / mL, ginkgolide B 10 μg / mL, ginkgolide C 14 μg / mL, ginsenoside F11 8 μg / mL, ginsenoside Rb1 10 μg / mL, ginsenoside Re 10 μg / mL and ginsenoside Rg1 14 μg / mL;

[0075] S3: The reference substance solution and the test sample solution were determined using a liquid chromatograph to obtain a chromatogram;

[0076] The chromatographic conditions were as follows:

[0077] Chromatographic column: USHA C18, size 2.1 mm x 50 mm, filler particle size 1.8 μm;

[0078] Mobile phase:

[0079] Mobile phase A: a mixed solution of acetonitrile and chloroform, the volume ratio of the two was 9:1;

[0080] Mobile phase B: a mixed solution of 0.25wt% phosphoric acid solution and 0.01wt% acetic acid solution, with a volume ratio of 4:1;

[0081] Flow rate: 1 mL·min -1 ;

[0082] Column temperature: 35℃;

[0083] Injection volume: 10 μL;

[0084] Detection wavelength: 290 nm;

[0085] The elution mode was gradient elution, and the elution gradient was as follows:

[0086] Table 1. Elution gradient

[0087] Time / min Mobile phase A / Vt% Mobile phase B / Vt% 0 10 90 5 10 90 15 14 86 20 25 75 35 30 70 50 30 70 60 78 22 70 78 22

[0088] The information of the obtained spectrum is shown in Table 2 as follows:

[0089] Table 2. Spectrum information

[0090] Sample name Peak no. Retention time / min Peak area Bilobanin 1 22.821 13245 Ginsenoside Rg1 2 24.315 8045 Ginsenoside Re 3 28.059 53147 Ginkgolide C 4 32.078 9683 Ginsenoside F11 5 35.278 11257 Ginsenoside Rb1 6 42.182 103284 Ginkgolide A 7 44.239 10598 Ginkgolide B 8 46.855 9178

[0091] Example 2

[0092] Different from Example 1, the detection wavelengths were 280 nm, 300 nm and 310 nm respectively, and the rest were the same. The results showed that the characteristic peaks of the ginkgo and ginseng preparation could also be separated at the detection wavelengths of 280 nm, 300 nm and 310 nm, but the peaks were more complete and the characteristic peaks were more obvious at the detection wavelength of 290 nm.

[0093] Example 3

[0094] Different from Example 1, the experiments were carried out at column temperatures of 30℃ and 40℃ respectively, and the rest were the same. The results showed that the separation degree of each main chromatographic peak was best and the peak shape was best at 35℃.

[0095] Example 4

[0096] Different from Example 1, the experiments were carried out at flow rates of 0.8 mL·min -1 , 0.9 mL·min -1 , 1.1 mL·min -1 , 1.2 mL·min -1 respectively, and the rest were the same. The results showed that the separation degree of each main chromatographic peak was best and the peak shape was best at a flow rate of 1.0 mL·min -1 .

[0097] Comparative Examples 1-6

[0098] Comparative Example 1-Comparative Example 6 differ from Example 1 in that only the solvent in S1 is changed, and the rest of the steps are the same. The content determination results are shown in Table 3 below.

[0099] Table 3. Effect of extraction solvent on content of each component

[0100]

[0101]

[0102] Comparative Example 7

[0103] Comparative Example 7 differs from Example 1 in that only the gradient elution procedure is changed, and the rest is the same.

[0104] The gradient elution procedure is shown below.

[0105] Table 4. Elution gradient

[0106] Time / min Mobile phase A / Vt% Mobile phase B / Vt% 0 25 75 15 35 65 40 45 55 50 50 50 70 60 60

[0107] Comparative Example 8

[0108] Comparative Example 8 differs from Example 1 in that only the mobile phase A is changed to acetonitrile, and the rest is the same.

[0109] Comparative Example 9

[0110] Comparative Example 9 differs from Example 1 in that only the mobile phase A is changed to chloroform, and the rest is the same.

[0111] Comparative Example 10

[0112] Comparative Example 10 differs from Example 1 in that only the mobile phase A is changed to methanol, and the rest is the same.

[0113] Comparative Example 11

[0114] Comparative Example 11 differs from Example 1 in that only the mobile phase B is changed to a 0.25wt% phosphoric acid solution, and the rest is the same.

[0115] Comparative Example 12

[0116] Comparative Example 12 differs from Example 1 in that only the mobile phase B is changed to a 0.01wt% sulfuric acid solution, and the rest is the same.

[0117] Detection Example

[0118] According to the detection method of Example 1, the specificity, linearity, precision, stability, repeatability and detection limit were investigated.

[0119] 1. Specificity

[0120] Accurately pipette 10 μL of the blank solvent and 10 μL of the test sample solution into the liquid chromatograph, respectively, and determine, to obtain.

[0121] Results: The blank solvent has no interference with the test sample.

[0122] 2. Linear relationship

[0123] Accurately pipette the control substances bilobalide, ginkgolide A, ginkgolide B, ginkgolide C, ginsenoside F11, ginsenoside Rbl, ginsenoside Re and ginsenoside Rgl into a solvent to prepare a control substance mixture solution with a certain concentration gradient; the solvent is a mixture of 85% (by volume) methanol solution and acetonitrile; the volume ratio of the 85% (by volume) methanol solution and acetonitrile is 10:1. Take 10 μL of the control substance mixture solution with low to high concentrations, respectively, and determine to investigate the linear relationship between the concentration (μg / mL) of each component and the corresponding peak area. The results show that the control substance concentration of bilobalide, ginkgolide A, ginkgolide B, ginkgolide C, ginsenoside F11, ginsenoside Rbl, ginsenoside Re and ginsenoside Rgl has a good linear relationship with the corresponding area, and the linear range of the sample amount of each component meets the detection requirements. The correlation coefficient R = 0.9999. 2

[0124] 3. Precision

[0125] Take the same sample of ginkgo and ginseng preparation to prepare a test sample solution with a concentration of 1 g / 50 mL, continuously inject 6 times, 210 μL each time, and record the retention time and peak area of peaks 1, 2, 3, 4, 5, 6, 7 and 8, respectively, and calculate the relative standard deviation RSD of the retention time and peak area of each peak. The RSD of the retention time of each peak is 0.08%-0.15%, and the RSD of the peak area is 0.11%-0.25%, both less than 3%, indicating that the precision of the instrument is good. The calculation results are shown in Table 5.

[0126] Table 5. Precision results

[0127]

[0128]

[0129] 4. Stability

[0130] According to the test sample preparation method of Example 1, the retention time of the same sample was determined at 0, 4, 8, 12, 36 and 48 h, respectively, and the RSD% was 0.18%-0.86%, indicating that the sample solution has good stability within 48 h. The results are shown in Table 6. ​

[0131] Table 6. Stability results

[0132]

[0133] 5. Reproducibility

[0134] According to the test sample preparation method of Example 1, 6 test sample solutions were prepared in parallel for the same batch of samples, and the content was determined. The results showed that the RSD% was 0.45%-0.92%, indicating that the method had good reproducibility. The results are shown in Table 7 below.

[0135] Table 7. Reproducibility results

[0136]

[0137] According to the detection method in the detection example, the linear correlation coefficient, precision, stability, and reproducibility of Example 1 and Comparative Examples 7-12 were detected, and the results are shown in Tables 8-11 below.

[0138] Table 8. Linear correlation coefficient R of Example 1 and Comparative Examples 7-12 2 Comparison (%)

[0139] Component Example 1 Comparative example 7 Comparative example 8 Comparative example 9 Comparative example 10 Comparative example 11 Comparative example 12 Bilobanin 0.9999 0.9991 0.9992 0.9991 0.9990 0.9990 0.9990 Ginsenoside Rg1 0.9999 0.9991 0.9990 0.9990 0.9993 0.9991 0.9995 Ginsenoside Re 0.9999 0.9994 0.9991 0.9992 0.9991 0.9990 0.9991 Ginkgolide C 0.9999 0.9992 0.9991 0.9992 0.9991 0.9990 0.9990 Ginsenoside F11 0.9999 0.9990 0.9991 0.9994 0.9990 0.9991 0.9992 Ginsenoside Rb1 0.9999 0.9991 0.9992 0.9990 0.9994 0.9991 0.9990 Ginkgolide A 0.9999 0.9992 0.9992 0.9991 0.9990 0.9991 0.9990 Ginkgolide B 0.9999 0.9990 0.9992 0.9991 0.9990 0.9991 0.9990

[0140] Table 9. Precision RSD (peak area) of Example 1 and Comparative Examples 7-12 Comparison (%)

[0141]

[0142]

[0143] Table 10. Stability RSD (retention time) of Example 1 and Comparative Examples 7-12 Comparison (%)

[0144] Component Example 1 Comparative example 7 Comparative example 8 Comparative example 9 Comparative example 10 Comparative example 11 Comparative example 12 Bilobanin 0.21 3.4 3.1 2.9 2.8 2.1 2.7 Ginsenoside Rg1 0.24 3.8 3.4 3.2 2.9 3.0 3.3 Ginsenoside Re 0.56 3.2 3.5 3.4 4.0 4.2 3.1 Ginkgolide C 0.86 5.1 5.5 5.3 4.9 5.0 4.8 Ginsenoside F11 0.18 2.1 2.2 2.5 1.9 2.0 2.4 Ginsenoside Rb1 0.41 3.1 2.8 2.9 2.5 2.4 2.7 Ginkgolide A 0.18 2.5 2.1 2.4 2.0 2.9 2.5 Ginkgolide B 0.81 4.9 4.8 4.5 3.6 3.5 4.0

[0145] Table 11. Reproducibility RSD (peak area) of Example 1 and Comparative Examples 7-12 Comparison (%)

[0146]

[0147]

[0148] Finally, it should be noted that the above content is only used to illustrate the technical solutions of the present application, and is not a limitation on the protection scope of the present application. Simple modifications or equivalent replacements of the technical solutions of the present application made by those skilled in the art do not deviate from the essence and scope of the technical solutions of the present application.

Claims

1. A quality detection method of a ginkgo ginseng preparation, characterized in that, Comprising the following steps: S1: Preparation of test solution: Take ginkgo ginseng preparation, crush, sieve, weigh, add solvent for extraction, filter membrane filtration, filter dry, add methanol to the residue, dissolve, constant volume, get test solution; The solvent is a mixture of n-butanol, methanol and ethyl acetate; The volume ratio of n-butanol, methanol and ethyl acetate is 8-12:5-7.5:0.5-1.5; The ginkgo ginseng preparation is ginkgo ginseng capsule and ginkgo ginseng granules; S2: Preparation of control solution: weigh the control substance ginkgolide, ginkgolide A, ginkgolide B, ginkgolide C, ginsenoside F11, ginsenoside Rb1, ginsenoside Re and ginsenoside Rg1, and mix with solvent to get control solution; S3: Use liquid chromatograph to determine the control solution and test solution, get chromatogram; Chromatographic conditions are: Chromatographic column: non-polar reverse phase chromatographic column with octadecylsilane bonded silica gel as filler; Mobile phase: Mobile phase A: acetonitrile and chloroform; Mobile phase B: 0.15-0.3wt% phosphoric acid solution and 0.01-0.015wt% acetic acid solution; Flow rate: 0.8-1.2 mL min -1 ; Column temperature: 30-40℃; Detection wavelength: 280-310nm; Elution mode is gradient elution, elution gradient is: 。 2. The quality detection method according to claim 1, characterized in that, In S1, the ratio of ginkgo ginseng preparation to solvent is 1:10-20g / mL; The extraction is ultrasonic extraction; The parameters of ultrasonic extraction are: ultrasonic power is 300-550W, frequency is 30-40kHz, time is 20-45min; The pore size of filter membrane is 0.2-0.35µm; The concentration of test solution is 1g / 50mL.

3. The quality detection method according to claim 1, characterized in that, In S2, the concentration of each control substance in the control solution is: ginkgolide 10-14µg / mL, ginkgolide A 6-14µg / mL, ginkgolide B 5-12µg / mL, ginkgolide C 1-160µg / mL, ginsenoside F11 7-15µg / mL, ginsenoside Rb1 80-130µg / mL, ginsenoside Re 50-80µg / mL and ginsenoside Rg1 1-10µg / mL.

4. The quality detection method of claim 1, wherein, In S2, the solvent is a mixture of 85% methanol solution and acetonitrile; The volume ratio of 85% methanol solution and acetonitrile is 8-12:

1.

5. The quality detection method of claim 1, wherein In S3, in the mobile phase A, the volume ratio of acetonitrile and chloroform is 8-12:1; The mobile phase B is: 0.25wt% phosphoric acid solution and 0.01wt% acetic acid solution; The volume ratio of 0.25wt% phosphoric acid solution and 0.01wt% acetic acid solution in the mobile phase B is 3-5:

1.

6. The quality detection method of claim 1, wherein In S3, the flow rate is 1 mL·min -1 ; the column temperature is 35 °C.

7. The application of the quality detection method of ginkgo ginseng preparation in the quality control of ginkgo ginseng preparation with ginkgo leaves and American ginseng as raw materials, the ginkgo ginseng preparation is ginkgo ginseng capsule and ginkgo ginseng granules.

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