CN1670524A - Method for measuring fingerprint pattern of compound salvia dropping pills - Google Patents
Method for measuring fingerprint pattern of compound salvia dropping pills Download PDFInfo
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- CN1670524A CN1670524A CN 200510055263 CN200510055263A CN1670524A CN 1670524 A CN1670524 A CN 1670524A CN 200510055263 CN200510055263 CN 200510055263 CN 200510055263 A CN200510055263 A CN 200510055263A CN 1670524 A CN1670524 A CN 1670524A
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Abstract
The invention relates to a method for measuring fingerprint pattern of compound salvia dropping pills, a method for establishing HPLC fingerprint pattern of compound salvia dropping pills by experiments and a standard fingerprint pattern thereof. A testing solution of compound salvia dropping pills is prepared firstly: 5-20 pellets of compound salvia dropping pills are taken and weighed precisely and placed into a volumetric flask of 10ml. Distilled water is added in with ultrasonic for 15min, then the sample is dissolved, volume metered, filtered to obtain the testing solution; gradient elution is adopted with mobile phase A to be 0.02% phosphoric acid solution and mobile phase B to be 80% acetonitrile phosphoric acid solution; flow rate is 1.000ml/min, detection wavelength is 280nm, column temperature is 30DEG C and injection volume is 10 mu l; the testing solution is determined by high performance liquid chromatography method to obtain the fingerprint pattern of compound salvia dropping pills. The method can obtain fingerprint pattern with high repeatability and be used as method for determining salvia dropping pills and quality control method for identifying compound salvia dropping pills.
Description
Technical field
The present invention relates to a kind of assay method of fingerprint pattern of compound salvia dropping pills, specifically use high performance liquid chromatography (HPLC) fingerprint spectrum method to measure a kind of method of effective constituent in the compound danshen dripping pills.
Background technology
Cardiovascular and cerebrovascular disease is the serious harm mankind's a common disease.In recent years, since the development of society, the variation of work, life, dietary structure and environment etc., and cardiovascular and cerebrovascular disease is in rising trend.Treatment for angiocardiopathy, though the action intensity of the single target spot of Chinese medicine is lower than Western medicine, but its multipath, many target spots, dynamically wholistic therapy, characteristic that toxic and side effect is little then are far from Western medicine and can reach, and the combined therapy effect of the Chinese patent drug of determined curative effect will surpass Western medicine.Compound red sage root preparation is used for treating cardiovascular and cerebrovascular disease more, for example Fufang Danshen Pian, compound danshen dripping pills, coronary heart disease drop pill etc.These compound red sage root preparations (all containing the red sage root, pseudo-ginseng) are different because of its prescription, and perhaps the formula rate difference is perhaps extracted the process for purification difference, and perhaps formulation difference, result of treatment be difference to some extent also.In addition, because the method for quality control of these compound red sage root preparations is comprehensive inadequately, be difficult to characterize their physicochemical characteristic comprehensively.Therefore, extraction process for purification, the method for quality control to compound red sage root preparation is modified into the problem into people's active research.
The red sage root is the dry root and rhizome of labiate red sage root Salvia miltiorrhiza Bge..All produce in most of area, the whole nation.Because the red sage root causes quality uneven because of kind, the place of production, picking time are different, thereby its manufactured goods quality of stability also is difficult to guarantee.At present, to the evaluation of the red sage root and compound preparation thereof, choose one, two active component or the index components of the red sage root often and carry out assay, and how much judge quality with its content.For example, with tanshinone IIA content (Chinese Pharmacopoeia 2000 version one one 58 pages) or content of Danshensu (Zhang Youqin etc., traditional Chinese medicine journal, 2000,28 (3): 68) wait the quality of differentiating red rooted salvia; Judge red sage root kind and place of production situation (Qiu Feijun, contemporary Chinese application pharmacy, 1998,15 (5): 16 with tanshinone; Hu Shilin etc., CHINA JOURNAL OF CHINESE MATERIA MEDICA, 1999,24 (12): 721); With content of Danshensu (Yan Changkai etc., Chinese Hospitals pharmaceutical journal, 2000,600), protocatechualdehyde content (Zheng end crystalline substance etc., Chinese Pharmaceutical Affairs, 2,000 20 (10):, 254) or tanshinone IIA content (Lin Weizhong etc. 14 (4):, Chinese patent drug, 766) etc. 2000,22 (11): the quality of differentiating compound red sage root preparation, differentiate the quality (Shao Shuijuan of the Fufang Danshen Pian that different manufacturers is produced with tanshinone IIA content, China's medicine company, 2000,9 (7): 27) etc.The chemical constitution of the known red sage root has tens kinds, and its liposoluble constituent mostly is quinoid reddish yellow material greatly, as Tanshinone I, IIA, IIB, and red sage root quinone A, B, C, red sage root acid potassium fat, isotanshinone I, II, Cryptotanshinone etc.Its water soluble ingredient mostly is phenol aldehyde, phenol acid, diterpenoid acid greatly, as succinic acid, salviandic acid A, B, C, and 3,4-dihydroxy-benzoic acid etc.In addition, also isolate cupreol, vitamin E etc. (Wang Baixiang chief editor, traditional Chinese medical science liver and bladder disease is learned, first published, Chinese Medicine science and technology publishing house,, 96 pages in 1993).Pseudo-ginseng is Araliaceae (Araliaceae) plant pseudo-ginseng Panaxnotoginseng (Burk.) F.H.Chen, dry root, main product in Yunnan, ground such as Guangxi and Sichuan, be the special product medicinal material of China's preciousness, conventional Chinese medicine.Its flavor is sweet, and little hardship is warm in nature, returns liver, kidney channel, has the effect of diffusing stasis of blood hemostasis, swelling and pain relieving, and tradition is used for the treatment of traumatic injury and various hemorrhagic disease.Studies show that pseudo-ginseng mainly contains chemical constitutions such as saponin, polysaccharide, amino acid, wherein saponin partly is the material base that pseudo-ginseng blood-circulation-invigovating stagnation resolvation effect is used, and is the main effective constituent of pseudo-ginseng.Notoginseng total saponin contains panaxoside R
B1, R
B2, R
c, R
d, R
e, R
f, R
G1, R
G2, B
H1, arasaponin R
1, R
2, R
3, R
4, R
6Deng kind of saponin component surplus 20.These compositions all belong to dammarane type [Dammarane type] tetracyclic triterpene saponin, wherein panaxoside R
B1, R
G1, arasaponin R
1Be 3 the highest compositions of content, arasaponin R
1It is the pseudo-ginseng compound of representative feature.
That traditional Chinese medicine fingerprint is meant is common in certain Chinese crude drug or the Chinese patent drug, have distinctive certain class or the chromatogram of number constituents or the collection of illustrative plates of spectrum.Do not have under the clear and definite situation in the present stage Effective Components of Chinese Herb overwhelming majority, traditional Chinese medicine fingerprint has great importance for the quality of effective control Chinese crude drug or Chinese patent drug.The Japan main manufacturing enterprise of Chinese prescription medicine just adopts the high-efficiency liquid-phase fingerprint control of quality in enterprises in the eighties in 20th century.Germany, France find that the medical function of ginkgo biloba p.e is extract gained material group's mass action result in the process that ginkgo biloba p.e is developed jointly, and to the quality control of such integral body, also adopt the high-efficiency liquid-phase fingerprint method.In the plant herbal medicine guide of formulating U.S. FDA recent years clearly the method for quality control (FDA.Guidance of Industry:Botanical Drug (Draft) .2000 August) of finger-print as the compounding substances group.Along with going deep into of research, it is found that, as the product of putting into practice of theory of traditional Chinese medical science, Chinese medicine, especially herbal mixture, wherein contained arbitrary composition all can not be represented its whole curative effect.People recognize that gradually the existing quality standard with reference to Western medicine (synthetic drug) quality control pattern can not reflect the quality of Chinese medicine inherence rightly.From development trend, from existing quality control pattern to a kind of comprehensive, macroscopic view, quantifiable discriminating combines with main active constituent content measuring is the trend that develops.
The act.std of medicine quality evaluated is to utilize spectrum or the discriminating of chromatogram means and measure a certain or several effective constituents, active component or index components, and the routine inspection project of pharmacopeia regulation.Record 602 kinds of medicinal materials and patent medicine kind altogether as Chinese Pharmacopoeia 2000 version [an one].Wherein have 992 thin-layer chromatographys to differentiate that 308 kinds have assay (volumetric method, spectroscopic methodology, liquid phase chromatography, vapor-phase chromatography and thin layer chromatography (TLC) scanning), most of kinds have general inspection item.Obviously, the setting of these quality standards is the patterns of having imitated chemicals.The German herbal medicine monograph that other country edits as the Chinese medicine in Britain, India, U.S.'s herbal medicine allusion quotation, the Pharmacopeia of Japan and German Commission E etc. has also adopted essentially identical content.For chemicals, its effective component is the simplification compound of clear in structure, and structure-activity relationship is clear and definite, and its content and purity are directly expressed it and effectively reached security.Yet the characteristics of middle medical drugs are compound compatibilities, any single effectively or the content of active component height all can not express its whole curative effect.For example, the contained Astragaloside IV (aastraga losideIV) of the Radix Astragali is the current discriminating of quality standard and the most common target of assay of being selected as, but not according to clearly getting in touch that the function that proves the Astragaloside IV and the Radix Astragali cures mainly.Equally, the coptis, golden cypress, radix berberidis all contain girder alkali, and be general all with its target as detection, completely different but three's function cures mainly.The situation of compound preparation is just complicated more.The traditional Chinese medical science is this not to be the comprehensive quality assessment means that man-to-man nonlinear theory and practice explanation traditional Chinese medicine quality should adopt certain macroscopic view.
Compound danshen dripping pills is to be the dropping pill formulation that primary raw material is made by the red sage root, pseudo-ginseng, be used for the treatment of cardiovascular and cerebrovascular disease, coronary heart disease, angina pectoris, myocardial ischemia, all kinds of diseases that microcirculation disorder caused etc. clinically, its result of treatment has obtained clinical checking, and whether can guarantee content of effective in the quality of medicine and the compound danshen dripping pills, be the basis of decision compound danshen dripping pills curative effect.If with one, the active component of two kind of red sage root illustrates the inherent quality of compound danshen dripping pills, has certain one-sidedness, said nothing of the index components of no drug effect.Control the effect of compound danshen dripping pills, only at one, two chemical constitutions characterize and control is not enough, must be controlled its material group integral body.So, except " micro-analysis ", also should characterize traditional Chinese medicine quality on the whole effectively with certain " macroanalysis " method.Finger-print is become a consensus of the international community at present as Chinese herbal medicine and extraction of substance amount control method thereof.Now, more to the assay method of active component such as tanshinone, danshensu etc. in the red sage root, to active component in the pseudo-ginseng such as arasaponin R
G1, panaxoside R
G1More Deng assay method, but can be that the method for building up of macroscopical finger-print of index does not appear in the newspapers to red sage root chemical composition the compound danshen dripping pills from more macroscopical angle how.
Summary of the invention
The assay method that the purpose of this invention is to provide a kind of compound danshen dripping pills macroscopic view finger-print, by this assay method, may command compound danshen dripping pills quality.
The present invention can implement through the following steps:
(a) preparation of compound danshen dripping pills test sample: get compound danshen dripping pills, put in the volumetric flask, the adding distil water ultrasonic dissolution, constant volume filters, and is test sample;
(b) chromatographic condition: chromatographic column is that octadecylsilane chemically bonded silica is a filler; Adopt gradient elution, mobile phase A is a phosphate aqueous solution; Mobile phase B is the acetonitrile phosphate aqueous solution, detects wavelength 274～286nm;
(c) measure: the accurate need testing solution of drawing injects liquid chromatograph, according to high effective liquid chromatography for measuring, obtains fingerprint pattern of compound salvia dropping pills.
Preferred the present invention can implement through the following steps: detect wavelength 277～283nm in described (a) step.
Further preferred fingerprint pattern of compound salvia dropping pills acquisition methods, method is as follows:
(a) preparation of compound danshen dripping pills need testing solution: get compound danshen dripping pills, the accurate title, decide, puts in 1～25ml volumetric flask, and the ultrasonic 5～30min of adding distil water, dissolving, constant volume filters, and is test sample;
(b) chromatographic condition: chromatographic column is that octadecylsilane chemically bonded silica is a filler; Adopt gradient elution, mobile phase A is 0.01% phosphate aqueous solution; Mobile phase B is 80% acetonitrile phosphate aqueous solution; The gradient elution program is as follows:
During 0min, mobile phase A is 90% 0.02% phosphate aqueous solution, and Mobile phase B is the phosphate aqueous solution of 10% 80% acetonitrile 0.02%;
During 8min, mobile phase A is 78% 0.02% phosphate aqueous solution, and Mobile phase B is the phosphate aqueous solution of 22% 80% acetonitrile 0.02%;
During 15min, mobile phase A is 74% 0.02% phosphate aqueous solution, and Mobile phase B is the phosphate aqueous solution of 26% 80% acetonitrile 0.02%;
During 55min, mobile phase A is 48% 0.02% phosphate aqueous solution, and Mobile phase B is the phosphate aqueous solution of 52% 80% acetonitrile 0.02%; Flow velocity 1.000ml/min detects wavelength 280nm, 30 ℃ of column temperatures, sampling volume 10 μ l;
(c) measure: the accurate need testing solution of drawing injects liquid chromatograph, according to high effective liquid chromatography for measuring, obtains fingerprint pattern of compound salvia dropping pills.
Best fingerprint pattern of compound salvia dropping pills acquisition methods, method is as follows:
(a) preparation of compound danshen dripping pills need testing solution: get 5～15 of compound danshen dripping pillses, the accurate title, decide, puts in the 10ml volumetric flask, and the ultrasonic 15min of adding distil water, dissolving, constant volume filters, and is test sample;
(b) chromatographic condition: chromatographic column is that octadecylsilane chemically bonded silica is a filler; Adopt gradient elution, mobile phase A is 0.02% phosphate aqueous solution; Mobile phase B is 80% acetonitrile phosphorus, 0.02% aqueous acid; The gradient elution program is as follows:
During 0min, mobile phase A is 90% 0.02% phosphate aqueous solution, and Mobile phase B is the phosphate aqueous solution of 10% 80% acetonitrile 0.02%;
During 8min, mobile phase A is 78% 0.02% phosphate aqueous solution, and Mobile phase B is the phosphate aqueous solution of 22% 80% acetonitrile 0.02%;
During 15min, mobile phase A is 74% 0.02% phosphate aqueous solution, and Mobile phase B is the phosphate aqueous solution of 26% 80% acetonitrile 0.02%;
During 55min, mobile phase A is 48% 0.02% phosphate aqueous solution, and Mobile phase B is the phosphate aqueous solution of 52% 80% acetonitrile 0.02%; Flow velocity 1.000ml/min detects wavelength 280nm, 30 ℃ of column temperatures, sampling volume 10 μ l;
(c) measure: the accurate need testing solution of drawing injects liquid chromatograph, and according to high effective liquid chromatography for measuring, the fingerprint pattern of compound salvia dropping pills absorption peak that obtains has 8, and the absorption peak that wherein unimodal area surpasses total peak area 2% has 8, is respectively:
No. 1 peak, average retention time RT is 6.04min, and RSD is 0.31%, and peak area is 1627.92, and RSD is 5.91%;
No. 2 peaks, average retention time RT is 9.90min, and RSD is 0.25%, and peak area is 2575.54, and RSD is 13.53%;
No. 3 peaks, average retention time RT is 16.89min, and RSD is 0.61%, and peak area is 366.89, and RSD is 10.92%;
No. 4 peaks, average retention time RT is 17.84min, and RSD is 0.07%, and peak area is 381.40, and RSD is 13.81%;
No. 5 peaks, average retention time RT is 20.31min, and RSD is 0.96%, and peak area is 186.08, and RSD is 12.04%;
No. 6 peaks, average retention time RT is 23.74min, and RSD is 0.76%, and peak area is 555.35, and RSD is 10.48%;
No. 7 peaks, average retention time RT is 27.73min, and RSD is 0.50%, and peak area is 281.91, and RSD is 18.08%;
No. 8 peaks, average retention time RT is 31.02min, and RSD is 1.18%, and peak area is 1852.33, and RSD is 14.84%.
In the described finger-print, absorption peak has 8 in the fingerprint pattern of compound salvia dropping pills, and the absorption peak that wherein unimodal area surpasses total peak area 5% has 4, is respectively:
No. 1 peak, average retention time RT is 6.04min, and RSD is 0.31%, and peak area is 1627.92, and RSD is 5.91%;
No. 2 peaks, average retention time RT is 9.90min, and RSD is 0.25%, and peak area is 2575.54, and RSD is 13.53%;
No. 6 peaks, average retention time RT is 23.74min, and RSD is 0.76%, and peak area is 555.35, and RSD is 10.48%;
No. 8 peaks, average retention time RT is 31.02min, and RSD is 1.18%, and peak area is 1852.33, and RSD is 14.84%.
In the described finger-print, absorption peak has 8 in the fingerprint pattern of compound salvia dropping pills, and the absorption peak that wherein unimodal area surpasses total peak area 10% has 3, is respectively:
No. 1 peak, average retention time RT is 6.04min, and RSD is 0.31%, and peak area is 1627.92, and RSD is 5.91%;
No. 2 peaks, average retention time RT is 9.90min, and RSD is 0.25%, and peak area is 2575.54, and RSD is 13.53%;
No. 8 peaks, average retention time RT is 31.02min, and RSD is 1.18%, and peak area is 1852.33, and RSD is 14.84%.
In the assay method of above-mentioned fingerprint pattern of compound salvia dropping pills, its configuration proportion that is used for the mobile phase A solution of gradient elution is to prepare by volume, and the configuration proportion of Mobile phase B solution is to prepare by volume.
The present invention measures the chemical constitution in red rooted salvia, the compound danshen dripping pills intermediate, and method is as follows:
Chemical composition high-efficiency liquid-phase fingerprint acquisition methods in the red rooted salvia, method is as follows:
The preparation of red rooted salvia test sample: get red rooted salvia and pulverize, put in the flask, add water, reflux is put coldly, collects phegma, will add water in the residue again, and reflux is put coldly, collects phegma, merges phegma twice, and constant volume filters, as test sample;
Chromatographic condition: chromatographic column is that octadecylsilane chemically bonded silica is a filler; Adopt gradient elution, mobile phase A is phosphoric acid～aqueous solution; Mobile phase B is the acetonitrile phosphate aqueous solution, and flow velocity 1.000ml/min detects wavelength 280nm, 30 ℃ of column temperatures;
Measure: the accurate need testing solution of drawing injects liquid chromatograph, according to high effective liquid chromatography for measuring, obtains the standard finger-print of Danshen component chemical constitution.
Chemical composition high-efficiency liquid-phase fingerprint acquisition methods in the preferred red rooted salvia, method is as follows:
The preparation of red rooted salvia test sample: get the red rooted salvia 2.5g of pulverizing, put in the flask, add 50ml water, reflux 1.5 hours is put coldly, collects phegma, 50ml water will be added in the residue again, reflux 1 hour is put coldly, collects phegma, merging two fries in shallow oil in phegma and the 100ml volumetric flask, constant volume filters, as test sample;
Chromatographic condition: chromatographic column is that octadecylsilane chemically bonded silica is a filler; Adopt gradient elution, mobile phase A is 0.02% phosphate aqueous solution mutually; Mobile phase B is the phosphate aqueous solution of 80% acetonitrile 0.02% mutually; The chromatogram flow phase gradient is as follows:
During 0min, mobile phase A is 90% 0.02% phosphate aqueous solution, and Mobile phase B is the phosphate aqueous solution of 10% 80% acetonitrile 0.02%;
During 8min, mobile phase A is 78% 0.02% phosphate aqueous solution, and Mobile phase B is the phosphate aqueous solution of 22% 80% acetonitrile 0.02%;
During 15min, mobile phase A is 74% 0.02% phosphate aqueous solution, and Mobile phase B is the phosphate aqueous solution of 26% 80% acetonitrile 0.02%;
During 55min, mobile phase A is 48% 0.02% phosphate aqueous solution, and Mobile phase B is the phosphate aqueous solution of 52% 80% acetonitrile 0.02%; Flow velocity 1.000ml/min detects wavelength 280nm, 30 ℃ of column temperatures, sampling volume 10 μ l;
Measure: the accurate need testing solution of drawing injects liquid chromatograph, according to high effective liquid chromatography for measuring, obtains the standard finger-print of Danshen component chemical constitution;
Danshen component chemical constitution absorption peak has 9 in the red rooted salvia, and the absorption peak that wherein unimodal area surpasses total peak area 2% has 9, is respectively:
No. 1 peak, average retention time RT is 5.99min, and RSD is 0.45%, and peak area is 784.93, and RSD is 7.34%;
No. 2 peaks, average retention time RT is 9.85min, and RSD is 0.47%, and peak area is 916.57, and RSD is 6.06%;
No. 3 peaks, average retention time RT is 20.13min, and RSD is 0.46%, and peak area is 778.87, and RSD is 8.78%;
No. 4 peaks, average retention time RT is 22.37min, and RSD is 0.77%, and peak area is 1165.13, and RSD is 7.60%;
No. 5 peaks, average retention time RT is 23.49min, and RSD is 0.45%, and peak area is 1076.7, and RSD is 3.70%;
No. 6 peaks, average retention time RT is 24.51min, and RSD is 0.46%, and peak area is 802.43, and RSD is 8.21%;
No. 7 peaks, average retention time RT is 27.26min, and RSD is 0.44%, and peak area is 9017.8, and RSD is 10.82%;
No. 8 peaks, average retention time RT is 29.71min, and RSD is 0.32%, and peak area is 539.37, and RSD is 13.30%;
No. 9 peaks, average retention time RT is 30.68min, and RSD is 0.29%, and peak area is 496.67, and RSD is 15.23%.
Danshen component chemical constitution absorption peak has 9 in the red rooted salvia, and the absorption peak that wherein unimodal area surpasses total peak area 5% has 7, is respectively:
No. 1 peak, average retention time RT is 5.99min, and RSD is 0.45%, and peak area is 784.93, and RSD is 7.34%;
No. 2 peaks, average retention time RT is 9.85min, and RSD is 0.47%, and peak area is 916.57, and RSD is 6.06%;
No. 3 peaks, average retention time RT is 20.13min, and RSD is 0.46%, and peak area is 778.87, and RSD is 8.78%;
No. 4 peaks, average retention time RT is 22.37min, and RSD is 0.77%, and peak area is 1165.13, and RSD is 7.60%;
No. 5 peaks, average retention time RT is 23.49min, and RSD is 0.45%, and peak area is 1076.7, and RSD is 3.70%;
No. 6 peaks, average retention time RT is 24.51min, and RSD is 0.46%, and peak area is 802.43, and RSD is 8.21%;
No. 7 peaks, average retention time RT is 27.26min, and RSD is 0.44%, and peak area is 9017.8, and RSD is 10.82%.
Danshen component chemical constitution absorption peak has 9 in the red rooted salvia, and the absorption peak that wherein unimodal area surpasses total peak area 10% has 1, is that No. 7 average retention time RT in peak are 27.26min, and RSD is 0.44%, and peak area is 9017.8, and RSD is 10.82%.
Red sage root chemical composition high-efficiency liquid-phase fingerprint acquisition methods in the compound danshen dripping pills intermediate, method is as follows:
The preparation of compound danshen dripping pills intermediate test sample: get Radix Salviae Miltiorrhizae extractum, place volumetric flask, the adding distil water ultrasonic dissolution, constant volume filters, and is test sample;
Chromatographic condition: chromatographic column is that octadecylsilane chemically bonded silica is a filler; Adopt gradient elution, mobile phase A is a phosphate aqueous solution; Mobile phase B is the acetonitrile phosphate aqueous solution, and flow velocity 1.000ml/min detects wavelength 280nm, 30 ℃ of column temperatures;
Measure: the accurate need testing solution of drawing injects liquid chromatograph, according to high effective liquid chromatography for measuring, obtains the standard finger-print of Danshen component chemical constitution in the compound danshen dripping pills;
Red sage root chemical composition high-efficiency liquid-phase fingerprint acquisition methods in the preferred compound danshen dripping pills intermediate, method is as follows:
The preparation of compound danshen dripping pills intermediate test sample: get Radix Salviae Miltiorrhizae extractum 0.1g, the accurate title, decide, puts in the 10ml volumetric flask, and the ultrasonic 15min of adding distil water, dissolving, constant volume filters, and is test sample;
Chromatographic condition: chromatographic column is that octadecylsilane chemically bonded silica is a filler; Adopt gradient elution, mobile phase A is 0.02% phosphate aqueous solution mutually; Mobile phase B is the phosphate aqueous solution of 80% acetonitrile 0.02% mutually; The chromatogram flow phase gradient is as follows:
During 0min, mobile phase A is 90% 0.02% phosphate aqueous solution, and Mobile phase B is the phosphate aqueous solution of 10% 80% acetonitrile 0.02%;
During 8min, mobile phase A is 78% 0.02% phosphate aqueous solution, and Mobile phase B is the phosphate aqueous solution of 22% 80% acetonitrile 0.02%;
During 15min, mobile phase A is 74% 0.02% phosphate aqueous solution, and Mobile phase B is the phosphate aqueous solution of 26% 80% acetonitrile 0.02%;
During 55min, mobile phase A is 48% 0.02% phosphate aqueous solution, and Mobile phase B is the phosphate aqueous solution of 52% 80% acetonitrile 0.02%; Flow velocity 1.000ml/min detects wavelength 280nm, 30 ℃ of column temperatures, sampling volume 10 μ l;
Measure: the accurate need testing solution of drawing injects liquid chromatograph, according to high effective liquid chromatography for measuring, obtains the standard finger-print of Danshen component chemical constitution in the compound danshen dripping pills;
In the described finger-print, Danshen component chemical constitution absorption peak has 8 in the compound danshen dripping pills intermediate, and the absorption peak that wherein unimodal area surpasses total peak area 2% has 8, is respectively:
No. 1 peak, average retention time RT is 6.12min, and RSD is 0.83%, and peak area is 2554.6, and RSD is 10.68%;
No. 2 peaks, average retention time RT is 10.00min, and RSD is 0.77%, and peak area is 4438.6, and RSD is 14.63%;
No. 3 peaks, average retention time RT is 15.96min, and RSD is 0.58%, and peak area is 740.16, and RSD is 13.18%;
No. 4 peaks, average retention time RT is 17.89min, and RSD is 1.17%, and peak area is 667.68, and RSD is 13.47%;
No. 5 peaks, average retention time RT is 20.27min, and RSD is 2.94%, and peak area is 654.73, and RSD is 15.01%;
No. 6 peaks, average retention time RT is 23.83min, and RSD is 0.88%, and peak area is 1140.51, and RSD is 16.45%;
No. 7 peaks, average retention time RT is 27.67min, and RSD is 0.61%, and peak area is 880.14, and RSD is 11.49%;
No. 8 peaks, average retention time RT is 30.93min, and RSD is 0.47%, and peak area is 2965.29, and RSD is 10.21%.
In the described finger-print, Danshen component chemical constitution absorption peak has 8 in the compound danshen dripping pills intermediate, and the absorption peak that wherein unimodal area surpasses total peak area 5% has 6, is respectively:
No. 1 peak, average retention time RT is 6.12min, and RSD is 0.83%, and peak area is 2554.6, and RSD is 10.68%;
No. 2 peaks, average retention time RT is 10.00min, and RSD is 0.77%, and peak area is 4438.6, and RSD is 14.63%;
No. 3 peaks, average retention time RT is 15.96min, and RSD is 0.58%, and peak area is 740.16, and RSD is 13.18%;
No. 6 peaks, average retention time RT is 23.83min, and RSD is 0.88%, and peak area is 1140.51, and RSD is 16.45%;
No. 7 peaks, average retention time RT is 27.67min, and RSD is 0.61%, and peak area is 880.14, and RSD is 11.49%;
No. 8 peaks, average retention time RT is 30.93min, and RSD is 0.47%, and peak area is 2965.29, and RSD is 10.21%.
In the described finger-print, Danshen component chemical constitution absorption peak has 8 in the compound danshen dripping pills intermediate, and the absorption peak that wherein unimodal area surpasses total peak area 10% has 3, is respectively:
No. 1 peak, average retention time RT is 6.12min, and RSD is 0.83%, and peak area is 2554.6, and RSD is 10.68%;
No. 2 peaks, average retention time RT is 10.00min, and RSD is 0.77%, and peak area is 4438.6, and RSD is 14.63%;
No. 8 peaks, average retention time RT is 30.93min, and RSD is 0.47%, and peak area is 2965.29, and RSD is 10.21%.
The present invention finds by the finger-print of measuring compound danshen dripping pills, compound danshen dripping pills intermediate, red rooted salvia, absorption peak quantity is almost completely identical among the three, illustrate that the chemical composition in the red rooted salvia almost completely is extracted in the compound danshen dripping pills, the finger-print of measuring the compound danshen dripping pills product can be used as the compound danshen dripping pills quality control standard, can objectively reflect the inherent composition of product have or not with and content, can control the quality of product comprehensively.
Advantage of the present invention is as follows:
(1). with main effective constituent red sage root chemical composition in the compound danshen dripping pills is the HPLC finger-print that index is set up, and is representing the most of pharmacologically active of compound danshen dripping pills, can characterize the quality of compound danshen dripping pills effectively.Thereby realize the chemical constitution of compound danshen dripping pills maximum possible is detected, help monitoring in all directions traditional Chinese medicine quality.
(2). do as a wholely to treat with each effective constituent fingerprint graph of the red sage root in the compound danshen dripping pills, pay attention to each front and back that constitute fingerprint characteristic peak order and mutual relationship, pay attention to whole facial feature, both avoided judging the one-sidedness of compound danshen dripping pills total quality that having reduced again was the possibility of the artificial processing of requisite quality because of only measuring one, two chemical constitution.The present invention provides new reference standard for quality complete, that accurately estimate compound danshen dripping pills, will be that the quality and the curative effect of principal ingredient prescribed preparation contributes with the red sage root, pseudo-ginseng for improving compound danshen dripping pills and other.
(3). the present invention has that method is easy, stable, precision is high, favorable reproducibility, the characteristics that are easy to grasp.
The invention provides a kind of detection method of compound danshen dripping pills, the present invention is by the resulting practicable method of a large amount of experiments, has repeatability.The repeatability of red sage root chemical composition high-efficiency liquid-phase fingerprint by red sage root chemical composition high-efficiency liquid-phase fingerprint, compound danshen dripping pills intermediate in high performance liquid chromatogram, the compound danshen dripping pills that obtained under the same test condition and red rooted salvia finger-print is good in the present invention, measure good reproducibility, therefore the fingerprint pattern of compound salvia dropping pills that can pass through the said determination method is set up is as standard finger-print, its assay method can be used as the standard finger-print that contains the red sage root, notoginseng preparations effective constituent determination, to differentiate its effective constituent.
To those skilled in the art, technology contents disclosed according to the present invention, those skilled in the art will very clear other embodiment of the present invention, and the embodiment of the invention is only as example.Under the situation of not violating purport of the present invention and scope, can carry out various changes and improvements to the present invention.For example, use the different measurement result that detecting instrument obtained possibilities different, but as long as use method of quality control of the present invention, all within protection domain of the present invention.
Description of drawings
Provide the contrast of the red sage root chemical composition HPLC finger-print of the finger-print of the red sage root, separate sources in red sage root finger-print, the compound danshen dripping pills in red rooted salvia finger-print, the compound danshen dripping pills intermediate below, be intended to further specify the present invention, but the present invention is not construed as limiting.
The finger-print of the red sage root in Fig. 1 red rooted salvia
The finger-print of the red sage root in Fig. 2 compound danshen dripping pills intermediate
The finger-print of the red sage root in Fig. 3 compound danshen dripping pills
The contrast of the red sage root chemical composition HPLC finger-print of Fig. 4 separate sources
Wherein: 1 is compound danshen dripping pills
2 is the compound danshen dripping pills intermediate
3 is red rooted salvia
Embodiment
The embodiment that enumerates the preparation aspect below further describes the present invention, and this embodiment only is used to illustrate the present invention, and the present invention is not construed as limiting.
Embodiment one (preparation example)
Take by weighing red sage root 41.06g, pseudo-ginseng 8.03g, the boiling secondary, the first time, 4 times of water gagings were 2 hours, the second time, 3 times of water gagings were 1 hour, filter, filtrate merges, when being concentrated into proportion and being 1.19-1.20 (75 ± 1 ℃), adding concentration is that 90% left and right sides ethanol to ethanol content is 65% (20 ℃), left standstill 12 hours, separation of supernatant reclaims ethanol, being concentrated into relative density of medicine liquid is 1.37 (55-60 ℃), gets Salvia miltiorrhiza and Panax notoginseng medicinal extract.Get above-mentioned Salvia miltiorrhiza and Panax notoginseng medicinal extract and borneol 0.46g, evenly be heated to 85 ℃ of temperature, change material after 80 minutes, move in the dropping-pill machine jar that jar temperature remains on 86 ℃ with polyglycol-6000 18g is mixed.In medicine liquid droplet to the 8 ℃ whiteruss, take out dripping pill, oil removing, screen cloth selects ball, promptly.
Embodiment two (preparation example)
Take by weighing red sage root 59.36g, pseudo-ginseng 6.38g, the boiling secondary, the first time, 4 times of water gagings were 2.5 hours, the second time, 3 times of water gagings were 1.5 hours, filter, filtrate merges, when being concentrated into proportion and being 1.19-1.20 (75 ± 1 ℃), adding concentration is that 85% left and right sides ethanol to ethanol content is 70% (20 ℃), left standstill 10 hours, separation of supernatant reclaims ethanol, being concentrated into relative density of medicine liquid is 1.35 (55-60 ℃), gets Salvia miltiorrhiza and Panax notoginseng medicinal extract.Get above-mentioned Salvia miltiorrhiza and Panax notoginseng medicinal extract and borneol 0.34g, evenly be heated to 89 ℃ of temperature, change material after 100 minutes, move in the dropping-pill machine jar that jar temperature remains on 85 ℃ with polyglycol-6000 23g is mixed.In medicine liquid droplet to the 8 ℃ methyl-silicone oil, take out dripping pill, oil removing, screen cloth selects ball, promptly.
Embodiment three (preparation example)
Take by weighing red sage root 31.12g, pseudo-ginseng 9.21g, add the NaOH of medicinal material total amount 0.5%, decoct secondary, the first time, 4 times of water gagings were 1.5 hours, and the second time, 3 times of water gagings were 1.5 hours, filtered, filtrate merges, when being concentrated into proportion and being 1.19-1.20 (75 ± 1 ℃), adding concentration is that 88% left and right sides ethanol to ethanol content is 66% (20 ℃), leaves standstill 10 hours, separation of supernatant, reclaim ethanol, being concentrated into relative density of medicine liquid is 1.40 (55-60 ℃), gets Salvia miltiorrhiza and Panax notoginseng medicinal extract.Get above-mentioned Salvia miltiorrhiza and Panax notoginseng medicinal extract and borneol 0.50g, sweet mellow wine 90g, mosatil 15g and distilled water 15ml, behind the said components mixing, powder-injection is made in freeze drying.
Embodiment four (preparation example)
Take by weighing red sage root 116.35g, pseudo-ginseng 58.21g, add the sodium bicarbonate of medicinal material total amount 2.0%, decoct secondary, the first time, 4 times of water gagings were 2 hours, and the second time, 3 times of water gagings were 1.5 hours, filtered, filtrate merges, when being concentrated into proportion and being 1.19-1.20 (75 ± 1 ℃), adding concentration is that 88% left and right sides ethanol to ethanol content is 66% (20 ℃), leaves standstill 10 hours, separation of supernatant, reclaim ethanol, being concentrated into relative density of medicine liquid is 1.40 (55-60 ℃), gets Salvia miltiorrhiza and Panax notoginseng medicinal extract.Get above-mentioned Salvia miltiorrhiza and Panax notoginseng medicinal extract and dalbergia heartwood oil 1.8g, mix, add 3% polyvidone ethanolic solution system softwood, cross 18 mesh sieve system particles with the 40g microcrystalline cellulose, 60 ℃ of dryings 35 minutes, whole grain, adding 4g talcum powder, mixing fills in capsule, promptly.
Embodiment five (preparation example)
Take by weighing red sage root 116.35g, pseudo-ginseng 58.21g, the boiling secondary, the first time, 4 times of water gagings were 2 hours, the second time, 3 times of water gagings were 1.5 hours, filter, filtrate merges, when being concentrated into proportion and being 1.19-1.20 (75 ± 1 ℃), adding concentration is that 88% left and right sides ethanol to ethanol content is 66% (20 ℃), left standstill 10 hours, separation of supernatant reclaims ethanol, being concentrated into relative density of medicine liquid is 1.40 (55-60 ℃), gets Salvia miltiorrhiza and Panax notoginseng medicinal extract.Get above-mentioned Salvia miltiorrhiza and Panax notoginseng medicinal extract and borneol 0.9g, mix with microcrystalline cellulose 120g, HPMC 40g, xylitol 5g, dolomol 2g, compressing tablet, promptly.
Embodiment six (preparation example)
Take by weighing red sage root 140.35g, pseudo-ginseng 36.42g, add the sodium bicarbonate of medicinal material total amount 2.5%, decoct secondary, the first time, 4 times of water gagings were 2 hours, and the second time, 3 times of water gagings were 1.5 hours, filtered, filtrate merges, when being concentrated into proportion and being 1.19-1.20 (75 ± 1 ℃), adding concentration is that 90% left and right sides ethanol to ethanol content is 65% (20 ℃), leaves standstill 8 hours, separation of supernatant, reclaim ethanol, being concentrated into relative density of medicine liquid is 1.35 (55-60 ℃), gets Salvia miltiorrhiza and Panax notoginseng medicinal extract.Get above-mentioned Salvia miltiorrhiza and Panax notoginseng medicinal extract and borneol 1.0g, mix, add 3% polyvidone ethanolic solution system softwood, cross 18 mesh sieve system particles with the 46g microcrystalline cellulose, 60 ℃ of dryings 30 minutes, whole grain, adding 4g talcum powder, mixing, compressing tablet, promptly.
Embodiment seven (compound danshen dripping pills Danshen component finger-print test example)
1, instrument and reagent
Instrument: adopt Agilent 1100 liquid chromatographies, comprise quaternary pump, online degasser, automatic sampler, DAD detecting device, column oven, Chemstation workstation; BS210S electronic balance (1/10
-4G) (Beijing Sai Duolisi company), METTLERAE240 electronic balance (1/10
-4G or 1/10
-5G) (plum Teller-Tuo benefit (Shanghai) Co., Ltd.), LD4-2 hydro-extractor (4000r/min) (Beijing Medical Centrifugal Machine Factory), digital display thermostat water bath (the long wind in Tianjin company limited), RE-52AA rotary evaporator (Shanghai Yarong Biochemical Instrument Plant), SHE-(III) circulation ability of swimming vacuum pump (Gongyi Ying Yu gives magnificent instrument plant), KQ-250B ultrasonic cleaner (Kunshan Ultrasonic Instruments Co., Ltd.), HENGAO T﹠amp; D filtrator (HENGGAO T﹠amp; D), synthon filtering membrane (aperture 0.45 μ m) (going up Haixing County inferior scavenging material factory);
Reagent: acetonitrile (chromatographically pure, U.S. Merck company), phosphoric acid (top grade is pure), Wahaha pure water.
2, test sample preparation:
Compound danshen dripping pills is for trying brilliant preparation: get 10 of embodiment one each batch compound danshen dripping pillses, accurate title is fixed, puts in the 10ml volumetric flask, and the ultrasonic 15min of adding distil water dissolves, and constant volume filters, and is test sample.
The preparation of compound danshen dripping pills intermediate test sample: get embodiment one each batch Salvia miltiorrhiza and Panax notoginseng medicinal extract 0.1g, the accurate title, decide, puts in the 10ml volumetric flask, and the ultrasonic 15min of adding distil water, dissolving, constant volume filters, and is test sample.
The preparation of red rooted salvia test sample: get red rooted salvia (pulverizing) 2.5g, put in the flask, add 50ml water, reflux 1.5 hours is put coldly, collects phegma.To add 50ml water in the residue again, reflux 1 hour is put coldly, collects phegma.Merge two and fry in shallow oil in phegma and the 100ml volumetric flask, constant volume filters, as test sample.
3, HPLC analysis condition
Agilent ZoRBAx SB-C
18(4.6 * 250mm, 5 μ m) chromatographic column, moving phase: A is 0.02% phosphate aqueous solution mutually; B is the phosphate aqueous solution of 80% acetonitrile 0.02% mutually.Flow velocity 1.000ml/min detects wavelength 280nm, 30 ℃ of column temperatures, sampling volume 10 μ l.
Chromatogram flow phase gradient such as following table:
Retention time mobile phase A (v/v) Mobile phase B (v/v)
0min?????????????????90％????????????????10％
8min?????????????????78％????????????????22％
15min????????????????74％????????????????26％
55min????????????????48％????????????????52％
The composition title:
| | | | Peak 4 |
| Danshensu | Protocatechualdehyde | Different alkannic acid A | Different alkannic |
| Peak | |||
| 5 | Peak 6 | Peak 7 | Peak 8 |
| Salvianolic acid D | Rosmarinic acid | Tanshin polyphenolic acid B | Salviandic acid A |
Data analysis
Amount to reply side's Radix Salviae Miltiorrhizae extractum surplus 200 is carried out red sage root fingerprint map analyzing respectively, its similarity is all more than 90%.Now gather the retention time of collection of illustrative plates, the mean value and the RSD value of peak area as follows:
Red sage root finger-print part
| Peak number | Average retention time | Retention time RSD% | Average peak area | Peak area RSD% | The unimodal number percent that accounts for total peak area |
| ????1 | ????6.12 | ????0.83 | ????2554.6 | ????10.68 | ????18.19％ |
| ????2 | ????10.00 | ????0.77 | ????4438.6 | ????14.63 | ????31.61％ |
| ????3 | ????15.96 | ????0.58 | ????740.16 | ????13.18 | ????5.27％ |
| ????4 | ????17.89 | ????1.17 | ????667.68 | ????13.47 | ????4.75％ |
| ????5 | ????20.27 | ????2.94 | ????654.73 | ????15.01 | ????4.66％ |
| ????6 | ????23.83 | ????0.88 | ????1140.51 | ????16.45 | ????8.12％ |
| ????7 | ????27.67 | ????0.61 | ????880.14 | ????11.49 | ????6.27％ |
| ????8 | ????30.93 | ????0.47 | ????2965.29 | ????10.21 | ????21.12％ |
In the described finger-print, Danshen component chemical constitution absorption peak has 8 in the compound danshen dripping pills intermediate, the absorption peak that wherein unimodal area surpasses total peak area 2% has 8, they are that No. 1 average retention time RT in peak is 6.12min, RSD is 0.83%, peak area is 2554.6, and RSD is 10.68%; No. 2 the average retention time RT in peak is 10.00min, and RSD is 0.77%, and peak area is 4438.6, and RSD is 14.63%; No. 3 the average retention time RT in peak is 15.96min, and RSD is 0.58%, and peak area is 740.16, and RSD is 13.18%; No. 4 the average retention time RT in peak is 17.89min, and RSD is 1.17%, and peak area is 667.68, and RSD is 13.47%; No. 5 the average retention time RT in peak is 20.27min, and RSD is 2.94%, and peak area is 654.73, and RSD is 15.01%; No. 6 the average retention time RT in peak is 23.83min, and RSD is 0.88%, and peak area is 1140.51, and RSD is 16.45%; No. 7 the average retention time RT in peak is 27.67min, and RSD is 0.61%, and peak area is 880.14, and RSD is 11.49%; No. 8 the average retention time RT in peak is 30.93min, and RSD is 0.47%, and peak area is 2965.29, and RSD is 10.21%.
In the described finger-print, Danshen component chemical constitution absorption peak has 8 in the compound danshen dripping pills intermediate, the absorption peak that wherein unimodal area surpasses total peak area 5% has 6, they are that No. 1 average retention time RT in peak is 6.12min, RSD is 0.83%, peak area is 2554.6, and RSD is 10.68%; No. 2 the average retention time RT in peak is 10.00min, and RSD is 0.77%, and peak area is 4438.6, and RSD is 14.63%; No. 3 the average retention time RT in peak is 15.96min, and RSD is 0.58%, and peak area is 740.16, and RSD is 13.18%; No. 6 the average retention time RT in peak is 23.83min, and RSD is 0.88%, and peak area is 1140.51, and RSD is 16.45%; No. 7 the average retention time RT in peak is 27.67min, and RSD is 0.61%, and peak area is 880.14, and RSD is 11.49%; No. 8 the average retention time RT in peak is 30.93min, and RSD is 0.47%, and peak area is 2965.29, and RSD is 10.21%.
In the described finger-print, Danshen component chemical constitution absorption peak has 8 in the compound danshen dripping pills intermediate, the absorption peak that wherein unimodal area surpasses total peak area 10% has 3, they are that No. 1 average retention time RT in peak is 6.12min, RSD is 0.83%, peak area is 2554.6, and RSD is 10.68%; No. 2 the average retention time RT in peak is 10.00min, and RSD is 0.77%, and peak area is 4438.6, and RSD is 14.63%; No. 8 the average retention time RT in peak is 30.93min, and RSD is 0.47%, and peak area is 2965.29, and RSD is 10.21%.
Amount to reply side's Danshen Root dropping ball surplus 200 is carried out red sage root fingerprint map analyzing respectively, its similarity is all more than 90%.Now gather the retention time of collection of illustrative plates, the mean value and the RSD value of peak area as follows:
The fingerprint pattern of compound salvia dropping pills part
| Peak number | Average retention time | Retention time RSD% | Average peak area | Peak area RSD% | The unimodal number percent that accounts for total peak area |
| ????1 | ????6.04 | ????0.31 | ??1627.92 | ????5.91 | ????20.80％ |
| ????2 | ????9.9 | ????0.25 | ??2575.54 | ????13.53 | ????32.90％ |
| ????3 | ????16.89 | ????0.61 | ??366.89 | ????10.92 | ????4.69％ |
| ????4 | ????17.84 | ????0.7 | ??381.4 | ????13.81 | ????4.87％ |
| ????5 | ????20.31 | ????0.96 | ????186.08 | ????12.04 | ????2.38％ |
| ????6 | ????23.74 | ????0.76 | ????555.35 | ????10.48 | ????7.09％ |
| ????7 | ????27.73 | ????0.5 | ????281.91 | ????18.08 | ????3.60％ |
| ????8 | ????31.02 | ????1.18 | ????1852.33 | ????14.84 | ????23.66％ |
In the foundation of reference fingerprint, there are 8 according to absorption peak in the finger-print of the contrast compound danshen dripping pills that high effective liquid chromatography for measuring obtained, the absorption peak that wherein unimodal area surpasses total peak area 10% has 3, they are that No. 1 average retention time RT in peak is 6.04min, RSD is 0.31%, peak area is 1627.92, and RSD is 5.91%; No. 2 the average retention time RT in peak is 9.90min, and RSD is 0.25%, and peak area is 2575.54, and RSD is 13.53%; No. 8 the average retention time RT in peak is 31.02min, and RSD is 1.18%, and peak area is 1852.33, and RSD is 14.84%;
In the foundation of reference fingerprint, there are 8 according to absorption peak in the finger-print of the contrast compound danshen dripping pills that high effective liquid chromatography for measuring obtained, the absorption peak that wherein unimodal area surpasses total peak area 5% has 4, is respectively:
No. 1 peak, average retention time RT is 6.04min, and RSD is 0.31%, and peak area is 1627.92, and RSD is 5.91%;
No. 2 peaks, average retention time RT is 9.90min, and RSD is 0.25%, and peak area is 2575.54, and RSD is 13.53%;
No. 6 peaks, average retention time RT is 23.74min, and RSD is 0.76%, and peak area is 555.35, and RSD is 10.48%;
No. 8 peaks, average retention time RT is 31.02min, and RSD is 1.18%, and peak area is 1852.33, and RSD is 14.84%;
In the foundation of reference fingerprint, there are 8 according to absorption peak in the finger-print of the contrast compound danshen dripping pills that high effective liquid chromatography for measuring obtained, the absorption peak that wherein unimodal area surpasses total peak area 2% has 8, is respectively:
No. 1 peak, average retention time RT is 6.04min, and RSD is 0.31%, and peak area is 1627.92, and RSD is 5.91%;
No. 2 peaks, average retention time RT is 9.90min, and RSD is 0.25%, and peak area is 2575.54, and RSD is 13.53%;
No. 3 peaks, average retention time RT is 16.89min, and RSD is 0.61%, and peak area is 366.89, and RSD is 10.92%;
No. 4 peaks, average retention time RT is 17.84min, and RSD is 0.07%, and peak area is 381.40, and RSD is 13.81%;
No. 5 peaks, average retention time RT is 20.31min, and RSD is 0.96%, and peak area is 186.08, and RSD is 12.04%;
No. 6 peaks, average retention time RT is 23.74min, and RSD is 0.76%, and peak area is 555.35, and RSD is 10.48%;
No. 7 peaks, average retention time RT is 27.73min, and RSD is 0.50%, and peak area is 281.91, and RSD is 18.08%;
No. 8 peaks, average retention time RT is 31.02min, and RSD is 1.18%, and peak area is 1852.33, and RSD is 14.84%.
Claims (5)
1. the assay method of a fingerprint pattern of compound salvia dropping pills, its feature comprises the steps:
(a) preparation of compound danshen dripping pills test sample: get compound danshen dripping pills, put in the volumetric flask, the adding distil water ultrasonic dissolution, constant volume filters, and is test sample;
(b) chromatographic condition: chromatographic column is that octadecylsilane chemically bonded silica is a filler; Adopt gradient elution, mobile phase A is a phosphate aqueous solution; Mobile phase B is the acetonitrile phosphate aqueous solution, detects wavelength 274～286nm;
(c) measure: the accurate need testing solution of drawing injects liquid chromatograph, according to high effective liquid chromatography for measuring, obtains fingerprint pattern of compound salvia dropping pills.
2. the assay method of fingerprint pattern of compound salvia dropping pills as claimed in claim 1 is characterized in that: detect wavelength 277～283nm in described (a) step.
3. the assay method of fingerprint pattern of compound salvia dropping pills as claimed in claim 1, its feature comprises the steps:
(a) preparation of compound danshen dripping pills need testing solution: get compound danshen dripping pills, the accurate title, decide, puts in 1～25ml volumetric flask, and the ultrasonic 5～30min of adding distil water, dissolving, constant volume filters, and is test sample;
(b) chromatographic condition: chromatographic column is that octadecylsilane chemically bonded silica is a filler; Adopt gradient elution, mobile phase A is 0.01% phosphate aqueous solution; Mobile phase B is 80% acetonitrile phosphate aqueous solution; The gradient elution program is as follows:
During 0min, mobile phase A is 90% 0.02% phosphate aqueous solution, and Mobile phase B is the phosphate aqueous solution of 10% 80% acetonitrile 0.02%;
During 8min, mobile phase A is 78% 0.02% phosphate aqueous solution, and Mobile phase B is the phosphate aqueous solution of 22% 80% acetonitrile 0.02%;
During 15min, mobile phase A is 74% 0.02% phosphate aqueous solution, and Mobile phase B is the phosphate aqueous solution of 26% 80% acetonitrile 0.02%;
During 55min, mobile phase A is 48% 0.02% phosphate aqueous solution, and Mobile phase B is the phosphate aqueous solution of 52% 80% acetonitrile 0.02%; Flow velocity 1.000ml/min detects wavelength 280nm, 30 ℃ of column temperatures, sampling volume 10 μ l;
(c) measure: the accurate need testing solution of drawing injects liquid chromatograph, according to high effective liquid chromatography for measuring, obtains fingerprint pattern of compound salvia dropping pills.
4. the assay method of fingerprint pattern of compound salvia dropping pills as claimed in claim 1, its feature comprises the steps:
(a) preparation of compound danshen dripping pills need testing solution: get 5～15 of compound danshen dripping pillses, the accurate title, decide, puts in the 10ml volumetric flask, and the ultrasonic 15min of adding distil water, dissolving, constant volume filters, and is test sample;
(b) chromatographic condition: chromatographic column is that octadecylsilane chemically bonded silica is a filler; Adopt gradient elution, mobile phase A is 0.02% phosphate aqueous solution; Mobile phase B is 80% acetonitrile phosphorus, 0.02% aqueous acid; The gradient elution program is as follows:
During 0min, mobile phase A is 90% 0.02% phosphate aqueous solution, and Mobile phase B is the phosphate aqueous solution of 10% 80% acetonitrile 0.02%;
During 8min, mobile phase A is 78% 0.02% phosphate aqueous solution, and Mobile phase B is the phosphate aqueous solution of 22% 80% acetonitrile 0.02%;
During 15min, mobile phase A is 74% 0.02% phosphate aqueous solution, and Mobile phase B is the phosphate aqueous solution of 26% 80% acetonitrile 0.02%;
During 55min, mobile phase A is 48% 0.02% phosphate aqueous solution, and Mobile phase B is the phosphate aqueous solution of 52% 80% acetonitrile 0.02%; Flow velocity 1.000ml/min detects wavelength 280nm, 30 ℃ of column temperatures, sampling volume 10 μ l;
(c) measure: the accurate need testing solution of drawing injects liquid chromatograph, according to high effective liquid chromatography for measuring, obtains fingerprint pattern of compound salvia dropping pills.
5. as the assay method of claim 1,2,3 or 4 described fingerprint pattern of compound salvia dropping pills, the configuration proportion that it is characterized in that mobile phase A solution is to prepare by volume, and the configuration proportion of Mobile phase B solution is to prepare by volume.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102621265A (en) * | 2012-03-27 | 2012-08-01 | 贵州景峰注射剂有限公司 | Method for measuring contents of multiple components in Shenxiong glucose injection |
| CN103424476A (en) * | 2012-05-25 | 2013-12-04 | 天津天士力之骄药业有限公司 | Method for simultaneously determining four water-soluble components in polydanshinolic acid |
| CN109406672A (en) * | 2018-11-20 | 2019-03-01 | 合肥创新医药技术有限公司 | A kind of fingerprint spectrum method using HPLC measurement Chinese medicine yiguan decoction |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| UA80674C2 (en) * | 2000-12-22 | 2007-10-25 | Herbal composition for angina pectoris (variants) | |
| CN1141575C (en) * | 2001-06-29 | 2004-03-10 | 天津市金士力药物研究开发有限公司 | Red sage medicine fingerprint establishing method and standard fingerprint atlas |
| CN1470868A (en) * | 2002-07-26 | 2004-01-28 | 天津市金士力药物研究开发有限公司 | Method for establishing fingerprint of red-rooted salvia root fat-soluble component and its standard map |
-
2005
- 2005-03-17 CN CNB2005100552633A patent/CN100412546C/en active Active
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102621265A (en) * | 2012-03-27 | 2012-08-01 | 贵州景峰注射剂有限公司 | Method for measuring contents of multiple components in Shenxiong glucose injection |
| CN102621265B (en) * | 2012-03-27 | 2014-09-24 | 贵州景峰注射剂有限公司 | Method for measuring contents of multiple components in Shenxiong glucose injection |
| CN103424476A (en) * | 2012-05-25 | 2013-12-04 | 天津天士力之骄药业有限公司 | Method for simultaneously determining four water-soluble components in polydanshinolic acid |
| CN103424476B (en) * | 2012-05-25 | 2016-08-17 | 天津天士力之骄药业有限公司 | Measure the method for 4 kinds of water soluble ingredients in poly phenolic acid of Radix Salviae Miltiorrhizae simultaneously |
| CN109406672A (en) * | 2018-11-20 | 2019-03-01 | 合肥创新医药技术有限公司 | A kind of fingerprint spectrum method using HPLC measurement Chinese medicine yiguan decoction |
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