CN102621246B - Method for simultaneous determination of contents of six active ingredients in Danhong injection using HPLC-DAD - Google Patents
Method for simultaneous determination of contents of six active ingredients in Danhong injection using HPLC-DAD Download PDFInfo
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- CN102621246B CN102621246B CN201210107254.4A CN201210107254A CN102621246B CN 102621246 B CN102621246 B CN 102621246B CN 201210107254 A CN201210107254 A CN 201210107254A CN 102621246 B CN102621246 B CN 102621246B
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Abstract
The invention relates to a method for simultaneous determination of contents of six active ingredients (sodium danshensu, protocatechualdehyde, coffeic acid, rosmarinic acid, salvianolic acid B and salvianolic acid A) in Danhong injection through using an HPLC-DAD (high performance liquid chromatography-diode array detector). The concrete technical scheme of the invention is as follows: preparing a sample solution and a control solution, carrying out gradient elution with an HPLC-DAD method, and measuring the contents of the six active ingredients (sodium danshensu, protocatechualdehyde, coffeic acid, rosmarinic acid, salvianolic acid B and salvianolic acid A) in Danhong. The method provided by the invention is simple, high in sensitivity and good in repeatability, solves the problem that in the existing Danhong injection, only the contents of two active ingredients are controlled, so that the quality issue of the Danhong injection cannot be comprehensively reflected, and provides more scientific basis for scientific evaluation and effective control of the quality of the Danhong injection.
Description
Technical field
The invention belongs to traditional Chinese medicine quality detection field, specifically a kind of HPLC-DAD of use measures the method for 6 kinds of active constituent contents in DANHONG ZHUSHEYE simultaneously.
Background technology
DANHONG ZHUSHEYE is the compound preparation being extracted by traditional blood-activating and stasis-removing red sage root, safflower, has promoting blood circulation and removing blood stasisly, improves microcirculation; reduce blood viscosity, accelerate velocity of blood flow, remove oxygen radical; Cell protection is avoided oxidative damage, suppresses the effects such as atherosclerotic.Be widely used in clinically coronary heart diseases and angina pectoris, myocardial infarction, acute cerebral infarction, chronic cardiopulmonary disease, Buerger's disease, atrophic gastritis and hypertensive nephropathy etc.The monarch drug in a prescription red sage root of DANHONG ZHUSHEYE is mainly containing water soluble ingredients such as danshensu, protocatechualdehyde, caffeic acid, Rosmarinic acid, tanshin polyphenolic acid B, salviandic acid As.In " national standard for traditional Chinese medicines compilation, internal medicine, feel concerned about fascicle ", promulgate in part and only Sodium Danshensu and 2 kinds of effective constituents of protocatechualdehyde are carried out to quality control about the national drug standards (trying) of DANHONG ZHUSHEYE.Due to ingredient more complicated in DANHONG ZHUSHEYE, be difficult to 6 kinds of effective constituents to separate with other compositions are good, reach the requirement of HPLC quantitative measurement.In view of this reason, have important practical significance therefore set up a kind of method of measuring 6 kinds of active constituent contents in DANHONG ZHUSHEYE simultaneously.
Summary of the invention
In order to solve the problems of the technologies described above, the invention provides a kind of HPLC-DAD of use and measure simultaneously the method for 6 kinds of active constituent contents in DANHONG ZHUSHEYE.Can effectively solve using danshensu, protocatechualdehyde, caffeic acid, Rosmarinic acid, tanshin polyphenolic acid B, salviandic acid A as index composition, carry out assay simultaneously, for the problem that DANHONG ZHUSHEYE quality standard lays the foundation, realize concrete technical scheme of the present invention and be:
Use HPLC-DAD to measure a method for 6 kinds of active constituent contents in DANHONG ZHUSHEYE simultaneously, it is characterized in that comprising the steps:
1) the accurate DANHONG ZHUSHEYE of drawing, adds ultrapure water dilution, shakes up, and filters through filter membrane, obtains need testing solution;
2) precision takes reference substance Sodium Danshensu, protocatechualdehyde, caffeic acid, Rosmarinic acid, tanshin polyphenolic acid B, salviandic acid A, puts respectively in volumetric flask, adds ultrapure water and dissolves, and dilution, mixes, and product stock solution in contrast refrigerates for subsequent use in 4 ℃ of refrigerators;
3) precision is drawn 6 kinds of reference substance stock solutions respectively again, adds ultrapure water dilution, accurately prepares the mixing reference substance solution of Sodium Danshensu, protocatechualdehyde, caffeic acid, Rosmarinic acid, tanshin polyphenolic acid B, salviandic acid A;
4) carry out the detection of HPLC-DAD method with following chromatographic condition: chromatographic column: Eclipse XDB-C
184.6 × 150 mm, 5 μ m; Mobile phase comprises mobile phase A: acetonitrile and Mobile phase B: the phosphate aqueous solution of volumn concentration 0.05%-0.1%; Adopt gradient elution mode, the volume ratio that acetonitrile accounts for mobile phase increases along with the increase of time in following ranges: 0-6 min, 5%-5%; 6-16 min, 5%-15%; 16-30 min, 15%-26%; 35-40 min, 26%-27%; DAD detecting device detects wavelength: detect Sodium Danshensu, protocatechualdehyde, tanshin polyphenolic acid B, salviandic acid A use 270-290 nm, detect caffeic acid, Rosmarinic acid use 320-340nm; Column temperature: 25-35 ℃; Flow velocity: 0.7-1.2 mLmin
-1;
5) get mixing reference substance solution, dilute different multiples with ultrapure water respectively, get above-mentioned dilution and mix reference substance solution and the former each sample introduction 10 μ l of reference substance solution that mix, record chromatogram and peak area, respectively take the peak area Y of 6 kinds of effective constituent chromatographic peaks as ordinate, with concentration X, μ gmL
-1for horizontal ordinate carries out linear regression, obtain regression equation and the related coefficient of typical curve;
6) get respectively the DANHONG ZHUSHEYE of different lot numbers, prepare sample solution by the preparation method of need testing solution, sample introduction 10 μ L respectively, measure peak area, every batch sample is measured 3 times, calculates the content of Sodium Danshensu, protocatechualdehyde, caffeic acid, Rosmarinic acid, tanshin polyphenolic acid B and salviandic acid A in different lot number DANHONG ZHUSHEYEs.
Described method, is characterized in that the accurate DANHONG ZHUSHEYE 2mL that draws in step 1), puts in 10mL volumetric flask, adds ultrapure water and is diluted to scale, shakes up, and filters through 0.45 μ m filter membrane, obtains need testing solution.
Described method, it is characterized in that step 2) in precision take reference substance Sodium Danshensu 6.55mg, protocatechualdehyde 5.05mg, caffeic acid 1.55mg, Rosmarinic acid 5.45mg, tanshin polyphenolic acid B 10.95mg, salviandic acid A 5.60mg, put respectively in 5mL volumetric flask, adding ultrapure water dissolves, be diluted to scale, mix, product stock solution in contrast refrigerates for subsequent use in 4 ℃ of refrigerators.
Described method, is characterized in that distinguishing accurate a certain amount of 6 kinds of reference substance stock solutions of drawing in step 3) again, adds ultrapure water dilution, accurately prepares Sodium Danshensu 1.310 mgmL
-1, protocatechualdehyde 0.101 mgmL
-1, caffeic acid 0.0041 mgmL
-1, Rosmarinic acid 0.109 mgmL
-1, tanshin polyphenolic acid B 0.219 mgmL
-1, salviandic acid A 3.360 mgmL
-1mixing reference substance solution.
Described method, the volumn concentration that it is characterized in that Mobile phase B phosphate aqueous solution in step 4) is 0.1%.
Described method, is characterized in that in step 4), DAD detecting device detects wavelength: detection Sodium Danshensu, protocatechualdehyde, tanshin polyphenolic acid B, salviandic acid A use 280 nm, detects caffeic acid, Rosmarinic acid use 330nm.
Described method, is characterized in that in step 4), column temperature is 30 ℃.
Described method, is characterized in that in step 4), flow velocity is 1.0 mLmin
-1.
Described method, it is characterized in that getting mixing reference substance solution in step 5), respectively with ultrapure water dilution 1.25,5,10,20,100 times, get above-mentioned 5 kinds of dilutions and mix reference substance solution and the former reference substance solution sample introduction 10 μ l separately that mix, record chromatogram and peak area, respectively take the peak area Y of 6 kinds of effective constituent chromatographic peaks as ordinate, with concentration X, μ gmL
-1for horizontal ordinate carries out linear regression, obtain regression equation and the related coefficient of typical curve.
The present invention adopts HPLC-DAD method, uses gradient elution to measure the content of Sodium Danshensu, protocatechualdehyde, caffeic acid, Rosmarinic acid, tanshin polyphenolic acid B and 6 kinds of effective constituents of salviandic acid A in DANHONG ZHUSHEYE.The linear relationship that calculates 6 kinds of effective constituents in DANHONG ZHUSHEYE, the results are shown in Table 1.
The linear relationship of 6 kinds of effective constituents of table 1 (
n=6)
Method of the present invention is easy, highly sensitive, favorable reproducibility, the quality assessment that has solved current DANHONG ZHUSHEYE can not reflect the problem of DANHONG ZHUSHEYE quality all sidedly, the quality of DANHONG ZHUSHEYE is carried out to the control of many indexs, for the quality of scientific evaluation and effective control DANHONG ZHUSHEYE provides more scientific foundation.
Accompanying drawing explanation
Fig. 1 is the ultraviolet-visible absorption spectroscopy figure of Sodium Danshensu reference substance;
Fig. 2 is the ultraviolet-visible absorption spectroscopy figure of protocatechualdehyde reference substance;
Fig. 3 is the ultraviolet-visible absorption spectroscopy figure of caffeic acid reference substance;
Fig. 4 is the ultraviolet-visible absorption spectroscopy figure of Rosmarinic acid reference substance;
Fig. 5 is the ultraviolet-visible absorption spectroscopy figure of tanshin polyphenolic acid B reference substance;
Fig. 6 is the ultraviolet-visible absorption spectroscopy figure of salviandic acid A reference substance;
Fig. 7 mixes the chromatogram of reference substance solution at 280nm;
Fig. 8 mixes the chromatogram of reference substance solution at 330nm;
Fig. 9 is the chromatogram of need testing solution (No.110934) at 280nm;
Figure 10 is the chromatogram of need testing solution (No.110934) at 330nm;
In Fig. 7 to Figure 10,1. Sodium Danshensu; 2. protocatechualdehyde; 3. caffeic acid; 4. Rosmarinic acid; 5.
Tanshin polyphenolic acid B; 6. salviandic acid A.
Embodiment
material
Agilent 1200 type highly effective liquid phase chromatographic systems (comprising G1311A quaternary gradient pump, G1316A column oven, G1315D diode array detector, G1315D DAD detecting device, the online degasser of G1322A and chem workstation).Ultrapure water instrument (Milipore company of the U.S.); XS105DualRange analytical balance (plum Teller-Tuo benefit Instrument Ltd.); Ultrasonic cleaner (Shanghai High Kudos Science Instrument Co., Ltd.).
DANHONG ZHUSHEYE (Heze Buchang Pharma Co., Ltd., specification 10 mL/ prop up); Sodium Danshensu reference substance (lot number 110855-200809), protocatechualdehyde reference substance (lot number 110810-201007), caffeic acid reference substance (lot number 20120211), Rosmarinic acid reference substance (lot number 111871-201102) are purchased from Nat'l Pharmaceutical & Biological Products Control Institute; Tanshin polyphenolic acid B reference substance (lot number 20110822), salviandic acid A reference substance (lot number 20120207) are purchased from Yuan Ye bio tech ltd, Shanghai.Acetonitrile (lot number 102489), methyl alcohol (lot number 101437) are purchased from Fisher company of the U.S., are chromatographically pure; Phosphoric acid, (lot number 76643827, Chemical Co., Ltd. of traditional Chinese medicines group) is pure for analyzing; Water is ultrapure water.
method and result
2.1accurate DANHONG ZHUSHEYE 2 mL that draw of preparation of need testing solution, put in 10 mL volumetric flasks, add ultrapure water and are diluted to scale, shake up, and filter through 0.45 μ m filter membrane, obtain need testing solution.
Mix the preparation of reference substance solution: precision takes reference substance Sodium Danshensu 6.55 mg, protocatechualdehyde 5.05 mg, caffeic acid 1.55 mg, Rosmarinic acid 5.45 mg, tanshin polyphenolic acid B 10.95 mg, salviandic acid A 5.60 mg, put respectively in 5 mL volumetric flasks, adding ultrapure water dissolves, be diluted to scale, mix, product stock solution in contrast refrigerates for subsequent use in 4 ℃ of refrigerators.
Precision is drawn a certain amount of 6 kinds of reference substance stock solutions respectively again, adds ultrapure water dilution, accurately prepares Sodium Danshensu 1.310 mgmL
-1, protocatechualdehyde 0.101 mgmL
-1, caffeic acid 0.0041 mgmL
-1, Rosmarinic acid 0.109 mgmL
-1, tanshin polyphenolic acid B 0.219 mgmL
-1, salviandic acid A 3.360 mgmL
-1mixing reference substance solution.
chromatographic conditioneclipse XDB-C
18chromatographic column (4.6 × 150 mm, 5 μ are m); Mobile phase adopts binary system, and A is acetonitrile, and B is 0.1% phosphate aqueous solution, and gradient elution mode is 0-6 min, 5%A; 6-16 min, 5%A-15%A; 16-30 min, 15%A-26%A; 30-40 min, 26%A-27%A; Column temperature is 30 ℃; Flow velocity is 1.0 mLmin
-1; Result obtains the ultraviolet-visible spectrum of 6 kinds of reference substances as shown in Fig. 1-Fig. 6, determine that by Fig. 1 and need testing solution chromatogram detecting wavelength is that 280 nm(measure Sodium Danshensu, protocatechualdehyde, tanshin polyphenolic acid B, salviandic acid A), 330 nm(measure caffeic acid, Rosmarinic acid).Under selected chromatographic condition, in sample liquid, 6 kinds of compositions obtain good separation with other peaks that coexist, and mix the chromatogram of reference substance solution and need testing solution and see Fig. 7-Figure 10.
2.4 linear relationships are investigated and are got mixing reference substance solution, respectively with ultrapure water dilution 1.25,5,10,20,100 times.Get above-mentioned 5 kinds of dilutions and mix reference substance solution and the former each sample introduction 10 μ l of reference substance solution that mix, record chromatogram and peak area, respectively take the peak area (Y) of 6 kinds of effective constituent chromatographic peaks as ordinate, with concentration (X, μ gmL
-1) for horizontal ordinate carries out linear regression, obtain regression equation and the related coefficient of typical curve, the results are shown in Table 1.
The linear relationship of 6 kinds of effective constituents of table 1 (
n=6)
2.5 precision tests are got mixing reference substance solution, by above-mentioned chromatographic condition, and sample introduction 10 μ l respectively, continuous sample introduction is measured 6 times, and the RSD that calculates 6 kinds of reference substance peak areas is respectively 0.14%, 0.24%, 0.06%, 0.08%, 0.06%, 0.23%.
2.6 replica tests are got 6 parts of same lot number DANHONG ZHUSHEYEs (No.110928), press 6 parts of test liquids of the parallel preparation of preparation method of need testing solution, with above-mentioned chromatographic condition analysis, every duplicate samples sample introduction 3 times, sample size 10 μ l, record chromatogram and peak area, in 6 parts of test liquids, the RSD of Sodium Danshensu, protocatechualdehyde, caffeic acid, Rosmarinic acid, tanshin polyphenolic acid B and salviandic acid A content is respectively 0.06%, 0.24%, 0.35%, 0.14%, 0.43%, 1.53% as a result.
Same need testing solution solution (No.110928) is got in 2.7 stability tests, 0,2,4,8,16,24 h sample introduction 10 μ L after preparing respectively, measure peak area, the RSD of result Sodium Danshensu, protocatechualdehyde, caffeic acid, Rosmarinic acid, tanshin polyphenolic acid B and salviandic acid A peak area is respectively 0.18%, 0.28%, 0.16%, 0.78%, 0.77%, 0.24%, shows that need testing solution is good at 24 h internal stabilities.
Accurate 6 parts of each 1 mL of DANHONG ZHUSHEYE (lot number 110928) that draw known content of 2.8 average recovery test, be placed in respectively 10 mL volumetric flasks, precision adds 100% Sodium Danshensu, protocatechualdehyde, caffeic acid, Rosmarinic acid, tanshin polyphenolic acid B and salviandic acid A reference substance, 6 parts of need testing solutions of parallel preparation, by above-mentioned chromatographic condition, each need testing solution sample introduction 10 μ L, measure the peak area of 6 kinds of effective constituents, calculate Sodium Danshensu, protocatechualdehyde, caffeic acid, Rosmarinic acid, the average recovery rate of tanshin polyphenolic acid B and salviandic acid A is respectively 98.98 ± 1.17%(RSD=1.19%), 100.86 ± 1.03%(RSD=1.02%), 100.44 ± 1.31%(RSD=1.30%), 98.73 ± 1.80%(RSD=1.82%), 101.35 ± 1.65%(RSD=1.63%), 100.17 ± 1.26%(RSD=1.26%).
2.9 sample sizes are measured the DANHONG ZHUSHEYE of getting respectively different lot numbers, prepare sample solution by the preparation method of need testing solution, and sample introduction 10 μ L respectively, measure peak area, and every batch sample is measured 3 times.The content that calculates Sodium Danshensu, protocatechualdehyde, caffeic acid, Rosmarinic acid, tanshin polyphenolic acid B and salviandic acid A in different lot number DANHONG ZHUSHEYEs, the results are shown in Table 2.
The content of 6 kinds of effective constituents in table 2 different batches DANHONG ZHUSHEYE (
n
= 3)
Claims (4)
1. use HPLC-DAD to measure a method for 6 kinds of active constituent contents in DANHONG ZHUSHEYE simultaneously, it is characterized in that comprising the steps:
1) the accurate DANHONG ZHUSHEYE 2mL that draws, puts in 10mL volumetric flask, adds ultrapure water and is diluted to scale, shakes up, and filters through 0.45 μ m filter membrane, obtains need testing solution;
2) precision takes reference substance Sodium Danshensu 6.55mg, protocatechualdehyde 5.05mg, caffeic acid 1.55mg, Rosmarinic acid 5.45mg, tanshin polyphenolic acid B 10.95mg, salviandic acid A 5.60mg, put respectively in 5mL volumetric flask, adding ultrapure water dissolves, be diluted to scale, mix, product stock solution in contrast refrigerates for subsequent use in 4 ℃ of refrigerators;
3) precision is drawn a certain amount of 6 kinds of reference substance stock solutions respectively again, adds ultrapure water dilution, accurately prepares Sodium Danshensu 1.310 mgmL
-1, protocatechualdehyde 0.101 mgmL
-1, caffeic acid 0.0041 mgmL
-1, Rosmarinic acid 0.109 mgmL
-1, tanshin polyphenolic acid B 0.219 mgmL
-1, salviandic acid A 3.360 mgmL
-1mixing reference substance solution;
4) carry out the detection of HPLC-DAD method with following chromatographic condition: chromatographic column: Eclipse XDB-C
184.6 × 150 mm, 5 μ m; Mobile phase comprises mobile phase A: acetonitrile and Mobile phase B: the phosphate aqueous solution that volumn concentration is 0.05%-0.1%; Adopt gradient elution mode, the percent by volume that acetonitrile accounts for mobile phase increases along with the increase of time in following ranges: 0-6 min, 5%-5%; 6-16 min, 5%-15%; 16-30 min, 15%-26%; 35-40 min, 26%-27%; DAD detecting device detects wavelength: detection Sodium Danshensu, protocatechualdehyde, tanshin polyphenolic acid B, salviandic acid A use 280 nm, detects caffeic acid, Rosmarinic acid use 330nm; Column temperature: 25-35 ℃; Flow velocity: 0.7-1.2 mLmin
-1;
5) get mixing reference substance solution, dilute different multiples with ultrapure water respectively, get above-mentioned dilution and mix reference substance solution and the former each sample introduction 10 μ l of reference substance solution that mix, record chromatogram and peak area, respectively take the peak area Y of 6 kinds of effective constituent chromatographic peaks as ordinate, with concentration X, μ gmL
-1for horizontal ordinate carries out linear regression, obtain regression equation and the related coefficient of typical curve;
6) get respectively the DANHONG ZHUSHEYE of different lot numbers, prepare sample solution by the preparation method of need testing solution, sample introduction 10 μ L respectively, measure peak area, every batch sample is measured 3 times, calculates the content of Sodium Danshensu, protocatechualdehyde, caffeic acid, Rosmarinic acid, tanshin polyphenolic acid B and salviandic acid A in different lot number DANHONG ZHUSHEYEs.
2. method claimed in claim 1, the volumn concentration the best that it is characterized in that Mobile phase B phosphate aqueous solution in step 4) is 0.1%.
3. the method for claim 1, is characterized in that in step 4), flow velocity the best is 1.0 mLmin
-1.
4. the method for claim 1, it is characterized in that getting mixing reference substance solution in step 5), respectively with ultrapure water dilution 1.25,5,10,20,100 times, get above-mentioned 5 kinds of dilutions and mix reference substance solution and the former each sample introduction 10 μ l of reference substance solution that mix, record chromatogram and peak area, respectively take the peak area Y of 6 kinds of effective constituent chromatographic peaks as ordinate, with concentration X, μ gmL
-1for horizontal ordinate carries out linear regression, obtain regression equation and the related coefficient of typical curve.
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| CN103913434A (en) * | 2014-04-04 | 2014-07-09 | 浙江大学 | Online method for detecting water sinking process of danhong injection |
| CN103940929B (en) * | 2014-05-05 | 2015-11-04 | 山东丹红制药有限公司 | A kind of detection method for the treatment of the traditional Chinese medicine injection of cardiovascular and cerebrovascular disease |
| CN104374844A (en) * | 2014-11-13 | 2015-02-25 | 贵州信邦制药股份有限公司 | Method for detecting content of water-soluble ingredients in salvia miltiorrhiza medicinal material and application of method |
| CN108037193B (en) * | 2017-11-01 | 2020-08-04 | 广西壮族自治区食品药品检验所 | Method for detecting compound salvia miltiorrhiza tablets by adopting HP L C-UV-E L SD method |
| CN110632190A (en) * | 2019-08-28 | 2019-12-31 | 湖南先伟实业有限公司 | Method for simultaneously measuring rosmarinic acid, carnosic acid and carnosol in rosemary |
| CN114295738B (en) * | 2021-12-08 | 2024-04-02 | 江苏弘典中药产业研究院有限公司 | Quality detection method of red sage leaf tea |
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