CN1679870A - Quality control of compound Danshen root drops - Google Patents
Quality control of compound Danshen root drops Download PDFInfo
- Publication number
- CN1679870A CN1679870A CN 200510054696 CN200510054696A CN1679870A CN 1679870 A CN1679870 A CN 1679870A CN 200510054696 CN200510054696 CN 200510054696 CN 200510054696 A CN200510054696 A CN 200510054696A CN 1679870 A CN1679870 A CN 1679870A
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- CN
- China
- Prior art keywords
- rsd
- fufang danshen
- peaks
- danshen diwan
- peak area
- Prior art date
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- 235000019165 vitamin E Nutrition 0.000 description 1
- 229940046009 vitamin E Drugs 0.000 description 1
- 239000011709 vitamin E Substances 0.000 description 1
- 239000000811 xylitol Substances 0.000 description 1
- 235000010447 xylitol Nutrition 0.000 description 1
- HEBKCHPVOIAQTA-SCDXWVJYSA-N xylitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)CO HEBKCHPVOIAQTA-SCDXWVJYSA-N 0.000 description 1
- 229960002675 xylitol Drugs 0.000 description 1
Images
Abstract
The invention relate to quality control method of compound Danshen root drops. The method comprises: measuring the fingerprint pattern of the compound Danshen root drops control sample by high efficiency liquid chromatography; measuring the fingerprint pattern of product to be measured of the compound Danshen root drops by the same method and in the same condition; comparing two results. When the absorption peak numbers of two results achieve the value described in the invention, the product to be measured is qualified.
Description
Technical field
The present invention relates to a kind of quality control of compound Danshen root drops, specifically utilize the quality of fingerprint atlas detection method control composite salvia dropping pill.
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 cardiovascular disease, 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 effects is little then are far from Western medicine and can reach, and the combined therapy effect of the Chinese patent medicine 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, FUFANG DANSHEN DIWAN, GUANXIN DANSHEN DIWAN etc.These compound red sage root preparations (all containing Radix Salviae Miltiorrhizae, Radix Notoginseng) are different because of its prescription, and perhaps the formula proportion difference is perhaps extracted the process for purification difference, perhaps dosage form difference, and therapeutic effect is 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.
Radix Salviae Miltiorrhizae is the dry root and rhizome of labiate Radix Salviae Miltiorrhizae Salvia miltiorrhiza Bge..All produce in most of area, the whole nation.Because Radix Salviae Miltiorrhizae causes quality uneven because of kind, the place of production, collection period are different, thereby its manufactured goods quality of stability also is difficult to guarantee.At present, to the evaluation of Radix Salviae Miltiorrhizae and compound preparation thereof, choose one, two active component or the index components of Radix Salviae Miltiorrhizae often and carry out assay, and how much judge quality with its content.For example, with tanshinone content (Chinese Pharmacopoeia 2000 version one one 58 pages) or content of Danshensu (Zhang Youqin etc., Chinese medicine journal, 2000,28 (3): 68) wait the quality of differentiating red rooted salvia; Judge Radix Salviae Miltiorrhizae kind and place of production situation (Qiu Feijun, contemporary Chinese application pharmacy, 1998,15 (5): 16 with TANSHINONES; 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 content (Lin Weizhong etc. 14 (4):, Chinese patent medicine, 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 content, China's Pharmaceutical, 2000,9 (7): 27) etc.The chemical constituent of known Radix Salviae Miltiorrhizae has tens kinds, and its liposoluble constituent mostly is quinoid reddish yellow material greatly, as Tanshinone I, IIA, IIB, and Radix Salviae Miltiorrhizae quinone A, B, C, Radix Salviae Miltiorrhizae acid potassium fat, iso tanshinone I, II, cryptotanshinone etc.Its water soluble ingredient mostly is phenol aldehyde, phenol acid, diterpenoid acid greatly, as succinic acid, salvianolic acid A, B, C, and 3,4-resorcylic acid etc.In addition, also isolate cupreol, vitamin E etc. (Wang Baixiang chief editor, traditional Chinese medical science liver-gallbladder disease is learned, front page, Chinese Medicine science and technology publishing house,, 96 pages in 1993).Radix Notoginseng is Araliaceae (Araliaceae) plant Radix Notoginseng Panaxnotoginseng (Burk.) F.H.Chen, dry root, main product in Yunnan, ground such as Guangxi and Sichuan, be the special product medical material of China's preciousness, conventional Chinese medicine.Its sweet in the mouth, little hardship, warm in nature, return liver, kidney channel, have the effect of dissipating blood stasis hemostasis, reducing swelling and alleviating pain, tradition is used for the treatment of traumatic injury and various hemorrhage.Studies show that Radix Notoginseng mainly contains chemical constituents such as Saponin, polysaccharide, aminoacid, wherein Saponin partly is the material base that pseudo-ginseng blood-circulation-invigovating blood stasis dispelling effect is used, and is the main effective ingredient of Radix Notoginseng.Radix Notoginseng total arasaponins contains ginsenoside 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 [Dammarsarane type] tetracyclic triterpene Saponin, wherein ginsenoside R
B1, R
G1, arasaponin R
1Be 3 the highest compositions of content, arasaponin R
1It is the Radix Notoginseng chemical compound of representative feature.
Chinese medicine fingerprint is meant chromatograph or spectrographic collection of illustrative plates common, that have distinctive certain class or number constituents in certain Chinese crude drug or the Chinese patent medicine.Do not have under the clear and definite situation in the present stage Effective Components of Chinese Herb overwhelming majority, Chinese medicine fingerprint has great importance for the quality of effective control Chinese crude drug or Chinese patent medicine.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 Folium Ginkgo extract is extract gained material group's mass action result in the process that Folium Ginkgo extract is developed jointly, and to the quality control of such integral body, also adopt the high-efficiency liquid-phase fingerprint method.In the plant medical herbs 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 printing 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 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 intrinsic quality of Chinese medicine rightly.From development trend, from existing quality control pattern to a kind of comprehensive, macroscopic, quantifiable discriminating combines with main active constituent content measuring is the trend that develops.
The working standard of medicine quality evaluated is to utilize spectrum or the discriminating of chromatograph means and measure a certain or several effective ingredient, active component or index components, and the routine examination project of pharmacopeia regulation.Record 602 kinds of medical 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, spectrographic method, liquid chromatography, gas chromatography and TLC scanning method), most of kinds have general inspection item.Obviously, the setting of these quality standards is the patterns of having imitated chemical drugs.The German medical herbs monograph that other country edits as the HANYAO in Britain, India, U.S.'s medical herbs allusion quotation, the Pharmacopeia of Japan and German Commission E etc. has also adopted essentially identical content.For chemical drugs, its active ingredient is the unification 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 safety.Yet the characteristics of middle medical drugs are compound compatibilities, and any single content height effective or active component all can not be expressed its whole curative effect.For example, the contained astragaloside (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 and the Radix Astragali cures mainly.Equally, Rhizoma Coptidis, Cortex Phellodendri, 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 that man-to-man nonlinear theory and practice explanation Chinese medicine quality should adopt certain macroscopic comprehensive quality evaluation means.
FUFANG DANSHEN DIWAN is to be the dropping pill formulation that primary raw material is made by Radix Salviae Miltiorrhizae, Radix Notoginseng, be used for the treatment of cardiovascular and cerebrovascular disease, coronary heart disease, angina pectoris, all kinds of diseases that myocardial ischemia, microcirculation disturbance caused etc. clinically, its therapeutic effect has obtained clinical checking, and whether can guarantee content of effective in the quality of medicine and the FUFANG DANSHEN DIWAN, be the basis of decision FUFANG DANSHEN DIWAN curative effect.If with one, the active component of two kind of Radix Salviae Miltiorrhizae illustrates the inherent quality of FUFANG DANSHEN DIWAN, has certain one-sidedness, said nothing of the index components of no drug effect.Control the effect of FUFANG DANSHEN DIWAN, only at one, two chemical constituents characterize and control is not enough, must be controlled its material group integral body.So, except " micro analysis ", also should characterize Chinese medicine quality on the whole effectively with certain " macroscopic analysis " method.Finger printing 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 TANSHINONES, danshensu etc. in the Radix Salviae Miltiorrhizae, to active component in the Radix Notoginseng such as arasaponin R
G1, ginsenoside R
G1More Deng assay method, but how can the macroscopic quality control method that the composite salvia dropping pill carries out quality control not appeared in the newspapers as yet from more macroscopic angle.
Summary of the invention
The method that the purpose of this invention is to provide a kind of FUFANG DANSHEN DIWAN quality control, by this kind method, the quality of may command composite salvia dropping pill.
The objective of the invention is to set up a kind of method of compound Chinese medicinal preparation quality control, the present invention is under certain condition by a large amount of experiments, finger printing and pseudo-ginseng finger printing, the FUFANG DANSHEN DIWAN intermediate finger printing of FUFANG DANSHEN DIWAN control sample are compared, observation is under identical chromatograph test condition, the repeatability of its absworption peak, and whether major part enters in FUFANG DANSHEN DIWAN intermediate and the FUFANG DANSHEN DIWAN control sample to determine effective chemical constituent in the pseudo-ginseng by finger printing.Prove by experiment, contain most of chemical constituent in the pseudo-ginseng among the present invention in the FUFANG DANSHEN DIWAN control sample, therefore measure the finger printing of Radix Salviae Miltiorrhizae chemical constituent in the FUFANG DANSHEN DIWAN, and itself and corresponding contrast fingerprint spectrogram compared, can control the quality of FUFANG DANSHEN DIWAN.
The present invention can implement through the following steps:
(a). the foundation of FUFANG DANSHEN DIWAN reference fingerprint
The preparation of FUFANG DANSHEN DIWAN control sample solution:
Claim FUFANG DANSHEN DIWAN, be dissolved in the ammonia of 1～20mL 1～8% ultrasonic dissolution, cross 0.30～0.60 μ m filter membrane, get the C-18 pillar that 2～10mL filtrate is crossed filler, flushing liquor is abandoned in methanol 1～8% ammonia spirit flushing of 5～40mL 8～35%, reuse 5～35ml washing, abandon water lotion, the reuse methanol-eluted fractions is collected methanol Shen and is taken off liquid in 1～15mL volumetric flask, standardize solution, centrifugal standby;
The mensuration of FUFANG DANSHEN DIWAN reference fingerprint:
Draw above-mentioned control sample solution and inject chromatograph of liquid, use high performance liquid chromatography to measure, obtain the FUFANG DANSHEN DIWAN reference fingerprint, chromatographic condition: chromatographic column is that octadecylsilane chemically bonded silica is a filler; Adopt gradient elution, mobile phase A is a glacial acetic acid aqueous solution, and Mobile phase B is the glacial acetic acid acetonitrile solution; Detect wavelength 200～210nm;
(b). the mensuration of FUFANG DANSHEN DIWAN product fingerprint collection of illustrative plates to be measured:
Get FUFANG DANSHEN DIWAN product to be measured, measure the finger printing of this product to be measured according to Step By Condition described in above-mentioned (a);
(c). described FUFANG DANSHEN DIWAN product fingerprint collection of illustrative plates to be measured and described FUFANG DANSHEN DIWAN reference fingerprint are compared, discern the quantity of its absworption peak, to determine whether product quality is qualified.
Preferred the present invention can implement through the following steps:
The preparation method of FUFANG DANSHEN DIWAN control sample solution is in described (a) step, claims FUFANG DANSHEN DIWAN, is dissolved in 5～15mL, 2～6% ammonia, ultrasonic dissolution is crossed 0.35～0.55 μ m filter membrane, gets the C-18 pillar that 2～10mL filtrate is crossed filler, methanol 2～6% ammonia spirits flushing of 10～30mL 10～30%, abandon flushing liquor, water lotion is abandoned in reuse 10～30ml washing, the reuse methanol-eluted fractions, collect meoh eluate in 1～10mL volumetric flask, standardize solution, centrifugal standby;
Chromatographic condition: chromatographic column is that octadecylsilane chemically bonded silica is a filler; Adopt gradient Shen to take off, mobile phase A is 0.01% glacial acetic acid aqueous solution mutually, and Mobile phase B is mutually for containing the acetonitrile solution of 0.01% glacial acetic acid; The gradient elution program is as follows:
In the time of 0 minute, mobile phase A is that 80% 0.01% glacial acetic acid aqueous solution, Mobile phase B are the acetonitrile solution of 20% 0.01% glacial acetic acid;
In the time of 15 minutes, mobile phase A is that 65% 0.01% glacial acetic acid aqueous solution, Mobile phase B are the acetonitrile solution of 35% 0.01% glacial acetic acid;
In the time of 25 minutes, mobile phase A is that 65% 0.01% glacial acetic acid aqueous solution, Mobile phase B are the acetonitrile solution of 35% 0.01% glacial acetic acid;
In the time of 40 minutes, mobile phase A is that 57% 0.01% glacial acetic acid aqueous solution, Mobile phase B are the acetonitrile solution of 43% 0.01% glacial acetic acid;
In the time of 50 minutes, mobile phase A is that 57% 0.01% glacial acetic acid aqueous solution, Mobile phase B are the acetonitrile solution of 43% 0.01% glacial acetic acid;
In the time of 65 minutes, mobile phase A is that 42% 0.01% glacial acetic acid aqueous solution, Mobile phase B are the acetonitrile solution of 58% 0.01% glacial acetic acid;
In the time of 75 minutes, mobile phase A is that 25% 0.01% glacial acetic acid aqueous solution, Mobile phase B are the acetonitrile solution of 75% 0.01% glacial acetic acid;
Sample size 5～45 μ L; Flow velocity 0.8mLmin
-1Detect wavelength 201～205nm; 25～35 ℃ of column temperatures.
Following method is adopted in the foundation of best FUFANG DANSHEN DIWAN standard finger-print:
The preparation method of FUFANG DANSHEN DIWAN control sample solution is in described (a) step, claims FUFANG DANSHEN DIWAN 0.4～1.5g, is dissolved in 10mL 4% ammonia, ultrasonic dissolution is crossed 0.45 μ m filter membrane, gets the C-18 pillar that 5mL filtrate is crossed the 500mg filler, flushing liquor is abandoned in the methanol 4% ammonia spirit flushing of 20mL 20%, reuse 20ml washing, abandon water lotion, the reuse methanol-eluted fractions is collected meoh eluate in 5mL volumetric flask, standardize solution, centrifugal standby, sample size 20 μ L;
Chromatographic condition: sample size 20 μ L; Flow velocity 0.8mLmin
-1Detect wavelength 203nm; 30 ℃ of column temperatures.
In the foundation of contrast fingerprint pattern of compound salvia dropping pills, the configuration proportion of its mobile phase A solution is to prepare by volume, and the configuration proportion of Mobile phase B solution is to prepare by volume.
In the foundation of FUFANG DANSHEN DIWAN reference fingerprint, according in the FUFANG DANSHEN DIWAN reference fingerprint that high effective liquid chromatography for measuring obtained 14 absworption peaks are arranged, the absworption peak that wherein unimodal area surpasses total peak area 10% has 3, is respectively:
No. 2 peaks, average retention time RT is 12.12min, and RSD is 0.34%, and peak area is 2723.73, and RSD is 12.11%;
No. 3 peaks, average retention time RT is 20.34min, and RSD is 0.23%, and peak area is 1684.49, and RSD is 18.59%;
No. 12 peaks, average retention time RT is 47.88min, and RSD is 0.25%, and peak area is 1547.80, and RSD is 13.25%.
In the foundation of FUFANG DANSHEN DIWAN reference fingerprint, according in the FUFANG DANSHEN DIWAN reference fingerprint that high effective liquid chromatography for measuring obtained 14 absworption peaks are arranged, the absworption peak that wherein unimodal area surpasses total peak area 5% has 7, is respectively:
No. 2 peaks, average retention time RT is 12.12min, and RSD is 0.34%, and peak area is 2723.73, and RSD is 12.11%;
No. 3 peaks, average retention time RT is 20.34min, and RSD is 0.23%, and peak area is 1684.49, and RSD is 18.59%;
No. 9 peaks, average retention time RT is 42.94min, and RSD is 0.21%, and peak area is 665.38, and RSD is 11.82%;
No. 11 peaks, average retention time RT is 45.68min, and RSD is 0.23%, and peak area is 947.39, and RSD is 16.06%;
No. 12 peaks, average retention time RT is 47.88min, and RSD is 0.25%, and peak area is 1547.80, and RSD is 13.25%;
No. 13 peaks, average retention time RT is 68.21min, and RSD is 0.13%, and peak area is 622.91, and RSD is 10.39%;
No. 14 peaks, average retention time RT is 69.43min, and RSD is 0.12%, and peak area is 820.24, and RSD is 12.94%.
In the foundation of FUFANG DANSHEN DIWAN reference fingerprint, according in the FUFANG DANSHEN DIWAN reference fingerprint that high effective liquid chromatography for measuring obtained 14 absworption peaks are arranged, the absworption peak that wherein unimodal area surpasses total peak area 2% has 13, is respectively;
No. 1 peak, average retention time RT is 10.87min, and RSD is 0.31%, and peak area is 506.92, and RSD is 13.03%;
No. 2 peaks, average retention time RT is 12.12min, and RSD is 0.34%, and peak area is 2723.73, and RSD is 12.11%;
No. 3 peaks, average retention time RT is 20.34min, and RSD is 0.23%, and peak area is 1684.49, and RSD is 18.59%;
No. 5 peaks, average retention time RT is 23.29min, and RSD is 0.25%, and peak area is 565.78, and RSD is 13.80%;
No. 6 peaks, average retention time RT is 24.48min, and RSD is 0.28%, and peak area is 309.39, and RSD is 18.98%;
No. 7 peaks, average retention time RT is 29.00min, and RSD is 0.62%, and peak area is 345.32, and RSD is 14.28%;
No. 8 peaks, average retention time RT is 41.21min, and RSD is 0.25%, and peak area is 436.06, and RSD is 10.88%;
No. 9 peaks, average retention time RT is 42.94min, and RSD is 0.21%, and peak area is 665.38, and RSD is 11.82%;
No. 10 peaks, average retention time RT is 44.16min, and RSD is 0.21%, and peak area is 472.84, and RSD is 14.59%;
No. 11 peaks, average retention time RT is 45.68min, and RSD is 0.23%, and peak area is 947.39, and RSD is 16.06%;
No. 12 peaks, average retention time RT is 47.88min, and RSD is 0.25%, and peak area is 1547.80, and RSD is 13.25%;
No. 13 peaks, average retention time RT is 68.21min, and RSD is 0.13%, and peak area is 622.91, and RSD is 10.39%;
No. 14 peaks, average retention time RT is 69.43min, and RSD is 0.12%, and peak area is 820.24, and RSD is 12.94%.
The present invention adopts the quality of following method control FUFANG DANSHEN DIWAN, get FUFANG DANSHEN DIWAN product to be measured, the identical method of the method for building up of employing and FUFANG DANSHEN DIWAN reference fingerprint, chromatographic condition, assay method is measured, obtain finger printing, FUFANG DANSHEN DIWAN product fingerprint collection of illustrative plates to be measured and FUFANG DANSHEN DIWAN reference fingerprint are compared, when the two finger printing has absworption peak identical more than 3 or 3, think the up-to-standard of described FUFANG DANSHEN DIWAN product to be measured.
Preferred FUFANG DANSHEN DIWAN product fingerprint collection of illustrative plates to be measured and the comparison of FUFANG DANSHEN DIWAN reference fingerprint when the two finger printing has absworption peak identical more than 5 or 5, are thought the up-to-standard of described FUFANG DANSHEN DIWAN product to be measured.
Further preferred FUFANG DANSHEN DIWAN product fingerprint collection of illustrative plates to be measured and the comparison of FUFANG DANSHEN DIWAN reference fingerprint when the two finger printing has absworption peak identical more than 7 or 7, are thought the up-to-standard of described FUFANG DANSHEN DIWAN product to be measured.
Further preferably get FUFANG DANSHEN DIWAN product fingerprint collection of illustrative plates to be measured and FUFANG DANSHEN DIWAN reference fingerprint relatively, when the two finger printing absworption peak surpasses absworption peak identical more than 13 or 7, think the up-to-standard of described FUFANG DANSHEN DIWAN product to be measured.
When best FUFANG DANSHEN DIWAN product fingerprint collection of illustrative plates to be measured and the comparison of FUFANG DANSHEN DIWAN reference fingerprint, the two finger printing have 14 identical absworption peaks, think the up-to-standard of described FUFANG DANSHEN DIWAN product to be measured.
The present invention measures Radix Notoginseng chemical constituent in pseudo-ginseng, the FUFANG DANSHEN DIWAN intermediate, and method is as follows:
Radix Notoginseng chemical constituent high-efficiency liquid-phase fingerprint acquisition methods in the pseudo-ginseng, method is as follows:
The preparation of pseudo-ginseng test sample: get it filled material in Backflow bottle, add the distilled water reflux, extract,, filter, add distilled water in the filtering residue, reflux, merging filtrate is dissolved in surely, and centrifugal filtration is standby;
The accurate need testing solution of drawing injects chromatograph of liquid, according to high effective liquid chromatography for measuring, obtains the finger printing of Radix Notoginseng component chemical composition;
In the described finger printing, the component chemical composition absworption peak of pseudo-ginseng test sample has 5, and the absworption peak that wherein unimodal area surpasses total peak area 10% has 3, is respectively:
No. 1 peak, average retention time RT is 10.81min, and RSD is 0.06%, and peak area is 539.57, and RSD is 17.73%;
No. 2 peaks, average retention time RT is 12.03min, and RSD is 0.02%, and peak area is 2482.50, and RSD is 8.74%;
No. 3 peaks, average retention time RT is 20.16min, and RSD is 0.11%, and peak area is 1514.5, and RSD is 12.02%.
Radix Notoginseng chemical constituent high-efficiency liquid-phase fingerprint acquisition methods in the preferred pseudo-ginseng, method is as follows:
The preparation of pseudo-ginseng test sample: take by weighing medical material 2.5g in Backflow bottle, add distilled water 50mL, refluxed 1.5 hours, filter, add the 50mL distilled water in the filtering residue, refluxed 1 hour, merging filtrate is dissolved in the 100mL measuring bottle surely, and centrifugal filtration is standby; Parallel 2 parts, sample size 10 μ L;
The accurate need testing solution of drawing injects chromatograph of liquid, according to high effective liquid chromatography for measuring, obtains the finger printing of Radix Notoginseng component chemical composition;
In the described finger printing, the component chemical composition absworption peak of pseudo-ginseng test sample has 5, and the absworption peak that wherein unimodal area surpasses total peak area 5% has 4, is respectively:
No. 1 peak, average retention time RT is 10.81min, and RSD is 0.06%, and peak area is 539.57, and RSD is 17.73%;
No. 2 peaks, average retention time RT is 12.03min, and RSD is 0.02%, and peak area is 2482.50, and RSD is 8.74%;
No. 3 peaks, average retention time RT is 20.16min, and RSD is 0.11%, and peak area is 1514.5, and RSD is 12.02%;
No. 5 peaks, average retention time RT is 28.42min, and RSD is 0.27%, and peak area is 356.20, and RSD is 15.30%.
Radix Notoginseng chemical constituent high-efficiency liquid-phase fingerprint acquisition methods in the best pseudo-ginseng, method is as follows:
The preparation of pseudo-ginseng test sample: take by weighing medical material 2.5g in Backflow bottle, add distilled water 50mL, refluxed 1.5 hours, filter, add the 50mL distilled water in the filtering residue, refluxed 1 hour, merging filtrate is dissolved in the 100mL measuring bottle surely, and centrifugal filtration is standby; Parallel 2 parts, sample size 10 μ L;
The accurate need testing solution of drawing injects chromatograph of liquid, according to high effective liquid chromatography for measuring, obtains the finger printing of Radix Notoginseng component chemical composition;
In the described finger printing, the component chemical composition absworption peak of pseudo-ginseng test sample has 5, and the absworption peak that wherein unimodal area surpasses total peak area 2% has 5, is respectively:
No. 1 peak, average retention time RT is 10.81min, and RSD is 0.06%, and peak area is 539.57, and RSD is 17.73%;
No. 2 peaks, average retention time RT is 12.03min, and RSD is 0.02%, and peak area is 2482.50, and RSD is 8.74%;
No. 3 peaks, average retention time RT is 20.16min, and RSD is 0.11%, and peak area is 1514.5, and RSD is 12.02%;
No. 4 peaks, average retention time RT is 23.04min, and RSD is 0.07%, and peak area is 250.63, and RSD is 18.25%;
No. 5 peaks, average retention time RT is 28.42min, and RSD is 0.27%, and peak area is 356.20, and RSD is 15.30%.
Radix Notoginseng chemical constituent high-efficiency liquid-phase fingerprint acquisition methods in the FUFANG DANSHEN DIWAN intermediate, method is as follows:
The preparation of FUFANG DANSHEN DIWAN intermediate test sample: take by weighing the FUFANG DANSHEN DIWAN intermediate,, be dissolved in the ammonia of 1～20mL 1～8%, ultrasonic dissolution is crossed 0.30～0.60 μ m filter membrane, gets the C-18 pillar that 2～10mL filtrate is crossed filler, flushing liquor is abandoned in methanol 1～8% ammonia spirit flushing of 5～40mL 8～35%, reuse 5～35ml washing, abandon water lotion, the reuse methanol-eluted fractions is collected meoh eluate in 1～15mL volumetric flask, standardize solution, centrifugal standby, parallel 2 parts, sample size 20 μ L;
Radix Notoginseng chemical constituent high-efficiency liquid-phase fingerprint acquisition methods in the preferred FUFANG DANSHEN DIWAN intermediate, method is as follows:
The preparation of FUFANG DANSHEN DIWAN intermediate test sample: take by weighing FUFANG DANSHEN DIWAN intermediate 0.2g, be dissolved in 5～15mL, 2～6% ammonia, ultrasonic dissolution, cross 0.35～0.55 μ m filter membrane, get the C-18 pillar that 2～10mL filtrate is crossed filler, methanol 2～6% ammonia spirits flushing of 10～30mL 10～30%, abandon flushing liquor, water lotion is abandoned in reuse 10～30ml washing, the reuse methanol-eluted fractions, collect meoh eluate in 1～10mL volumetric flask, standardize solution, centrifugal standby, parallel 2 parts, sample size 20 μ L;
Radix Notoginseng chemical constituent high-efficiency liquid-phase fingerprint acquisition methods in the best FUFANG DANSHEN DIWAN intermediate, method is as follows:
The preparation of FUFANG DANSHEN DIWAN intermediate test sample: take by weighing FUFANG DANSHEN DIWAN intermediate 0.1～0.5g, be dissolved in 10mL 4% ammonia, ultrasonic dissolution, cross 0.45 μ m filter membrane, get the C-18 pillar that 5mL filtrate is crossed the 500mg filler, the methanol 4% ammonia spirit flushing of 20mL 20%, abandon flushing liquor, water Shen liquid is abandoned in reuse 20ml washing, the reuse methanol-eluted fractions, collect meoh eluate in the 5mL volumetric flask, standardize solution, centrifugal standby, parallel 2 parts, sample size 20 μ L;
The accurate need testing solution of drawing injects chromatograph of liquid, according to high effective liquid chromatography for measuring, obtains the finger printing of Radix Notoginseng component chemical composition;
Radix Notoginseng component chemical composition absworption peak has 12 in the FUFANG DANSHEN DIWAN intermediate, and the absworption peak that wherein unimodal area surpasses total peak area 2% has 11, is respectively:
No. 1 peak, average retention time RT is 10.85min, and RSD is 0.08%, and peak area is 557.29, and RSD is 15.67%;
No. 2 peaks, average retention time RT is 12.10min, and RSD is 0.06%, and peak area is 2728.83, and RSD is 16.66%;
No. 3 peaks, average retention time RT is 20.33min, and RSD is 0.08%, and peak area is 3704.31, and RSD is 14.15%;
No. 4 peaks, average retention time RT is 23.86min, and RSD is 0.07%, and peak area is 272.69, and RSD is 12.54%;
No. 5 peaks, average retention time RT is 23.28min, and RSD is 0.08%, and peak area is 369.12, and RSD is 21.52%;
No. 7 peaks, average retention time RT is 28.82min, and RSD is 1.36%, and peak area is 289.16, and RSD is 17.71%;
No. 8 peaks, average retention time RT is 42.93min, and RSD is 0.07%, and peak area is 239.14, and RSD is 18.84%;
No. 9 peaks, average retention time RT is 45.66min, and RSD is 0.06%, and peak area is 445.17, and RSD is 19.56%;
No. 10 peaks, average retention time RT is 47.85min, and RSD is 0.06%, and peak area is 723.59, and RSD is 14.24%;
No. 11 peaks, average retention time RT is 68.17min, and RSD is 0.03%, and peak area is 407.66, and RSD is 10.86%;
No. 12 peaks, average retention time RT is 69.4min, and RSD is 0.03%, and peak area is 476.31, and RSD is 15.46%.
Radix Notoginseng component chemical composition absworption peak has 12 in the FUFANG DANSHEN DIWAN intermediate, and the absworption peak that wherein unimodal area surpasses total peak area 5% has 4, is respectively:
No. 1 peak, average retention time RT is 10.85min, and RSD is 0.08%, and peak area is 557.29, and RSD is 15.67%;
No. 2 peaks, average retention time RT is 12.10min, and RSD is 0.06%, and peak area is 2728.83, and RSD is 16.66%;
No. 3 peaks, average retention time RT is 20.33min, and RSD is 0.08%, and peak area is 3704.31, and RSD is 14.15%;
No. 10 peaks, average retention time RT is 47.85min, and RSD is 0.06%, and peak area is 723.59, and RSD is 14.24%.
Radix Notoginseng component chemical composition absworption peak has 12 in the FUFANG DANSHEN DIWAN intermediate, and the absworption peak that wherein unimodal area surpasses total peak area 10% has 2, is respectively:
No. 2 peaks, average retention time RT is 12.10min, and RSD is 0.06%, and peak area is 2728.83, and RSD is 16.66%;
No. 3 peaks, average retention time RT is 20.33min, and RSD is 0.08%, and peak area is 3704.31, and RSD is 14.15%;
No. 10 peaks, average retention time RT is 47.85min, and RSD is 0.06%, and peak area is 723.59, and RSD is 14.24%.
The present invention finds by the finger printing of measuring FUFANG DANSHEN DIWAN, FUFANG DANSHEN DIWAN intermediate, pseudo-ginseng, absworption peak quantity and incomplete same among the three, illustrate that the finger printing that adopts the FUFANG DANSHEN DIWAN product more can objectively reflect the having or not and content of product inherent composition than independent finger printing with the Radix Notoginseng composition as quality standard as the FUFANG DANSHEN DIWAN quality control standard, with the quality of comprehensive control product.
Advantage of the present invention is as follows:
(1). with main effective ingredient Radix Notoginseng chemical constituent in the FUFANG DANSHEN DIWAN is the HPLC standard finger-print that index is set up, and is representing the most of pharmacologically active of FUFANG DANSHEN DIWAN, can characterize the quality of FUFANG DANSHEN DIWAN effectively.Thereby realize the chemical constituent of FUFANG DANSHEN DIWAN maximum possible is detected, help monitoring in all directions Chinese medicine quality.
(2). each effective ingredient fingerprint graph of Radix Notoginseng in the FUFANG DANSHEN DIWAN is done as a wholely to treat, pay attention to each front and back that constitute fingerprint characteristic peak order and mutual relation, pay attention to whole facial feature, both avoided judging the one-sidedness of FUFANG DANSHEN DIWAN total quality that having reduced again was the probability of the artificial processing of requisite quality because of only measuring one, two chemical constituent.The present invention provides new reference standard for quality complete, that accurately estimate FUFANG DANSHEN DIWAN, will be that the quality and the curative effect of main component prescribed preparation contributes with Radix Salviae Miltiorrhizae, Radix Notoginseng for improving FUFANG DANSHEN DIWAN 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 authentication method of FUFANG DANSHEN DIWAN, the present invention is in the present invention by Radix Notoginseng chemical constituent high performance liquid chromatogram standard finger-print in high performance liquid chromatogram, the FUFANG DANSHEN DIWAN obtained under the same test condition by the resulting practicable method of a large amount of experiments, characteristics with 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 Radix Salviae Miltiorrhizae, notoginseng preparations effective constituent determination, to differentiate its effective ingredient.
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 Radix Notoginseng chemical constituent HPLC finger printing of finger printing, the separate sources of compound components of panax notoginseng in the finger printing, FUFANG DANSHEN DIWAN of compound components of panax notoginseng in pseudo-ginseng finger printing, the FUFANG DANSHEN DIWAN intermediate below, be intended to further specify the present invention, but the present invention is not construed as limiting.
The finger printing of Fig. 1 pseudo-ginseng compound components of panax notoginseng
The finger printing of compound components of panax notoginseng in Fig. 2 FUFANG DANSHEN DIWAN intermediate
The finger printing of compound components of panax notoginseng in Fig. 3 FUFANG DANSHEN DIWAN
The contrast of the Radix Notoginseng chemical constituent HPLC finger printing of Fig. 4 separate sources
Wherein: 1 is FUFANG DANSHEN DIWAN
2 is the FUFANG DANSHEN DIWAN intermediate
3 is pseudo-ginseng
The specific embodiment
The embodiment that enumerates the preparation aspect below further describes the present invention, and this embodiment only is used to the present invention is described and the present invention is not limited.
Embodiment one (preparation example)
Take by weighing Radix Salviae Miltiorrhizae 41.06g, Radix Notoginseng 8.03g, decoct with water 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 extractum.Get above-mentioned Salvia miltiorrhiza and Panax notoginseng extractum and Borneolum Syntheticum 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 Polyethylene Glycol-6000 18g is mixed.In medicine liquid droplet to the 8 ℃ liquid paraffin, take out drop pill, oil removing, screen cloth selects ball, promptly.
Embodiment two (preparation example)
Take by weighing Radix Salviae Miltiorrhizae 59.36g, Radix Notoginseng 6.38g, add the potassium carbonate of medical material total amount 1.0%, decoct secondary, the first time, 4 times of water gagings were 2.5 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 85% left and right sides ethanol to ethanol content is 70% (20 ℃), leaves standstill 10 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 extractum.Get above-mentioned Salvia miltiorrhiza and Panax notoginseng extractum and Borneolum Syntheticum 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 Polyethylene Glycol-6000 23g is mixed.In medicine liquid droplet to the 8 ℃ methyl-silicone oil, take out drop pill, oil removing, screen cloth selects ball, promptly.
Embodiment three (preparation example)
Take by weighing Radix Salviae Miltiorrhizae 31.12g, Radix Notoginseng 9.21g, add the sodium hydroxide of medical 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 extractum.Get above-mentioned Salvia miltiorrhiza and Panax notoginseng extractum and Borneolum Syntheticum 0.50g, mannitol 90g, calcium disodium edetate 15g and distilled water 15ml, behind the said components mixing, injectable powder is made in lyophilization.
Embodiment four (preparation example)
Take by weighing Radix Salviae Miltiorrhizae 116.35g, Radix Notoginseng 58.21g, decoct with water 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 extractum.Get above-mentioned Salvia miltiorrhiza and Panax notoginseng extractum and Lignum Dalbergiae Odoriferae oil 1.8g,, add 3% polyvidone alcoholic solution system soft material, cross 18 mesh sieve system granules with 40g microcrystalline Cellulose mix homogeneously, 60 ℃ of dryings 35 minutes, granulate, adding 4g Pulvis Talci, mixing fills in capsule, promptly.
Embodiment five (preparation example)
Take by weighing Radix Salviae Miltiorrhizae 116.35g, Radix Notoginseng 58.21g, add the sodium bicarbonate of medical 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 extractum.Get above-mentioned Salvia miltiorrhiza and Panax notoginseng extractum and Borneolum Syntheticum 0.9g, with microcrystalline Cellulose 120g, hydroxypropyl methylcellulose 40g, xylitol 5g, magnesium stearate 2g mix homogeneously, tabletting, promptly.
Embodiment six (preparation example)
Take by weighing Radix Salviae Miltiorrhizae 140.35g, Radix Notoginseng 36.42g, decoct with water 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 90% left and right sides ethanol to ethanol content is 65% (20 ℃), left standstill 8 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 extractum.Get above-mentioned Salvia miltiorrhiza and Panax notoginseng extractum and Borneolum Syntheticum 1.0g,, add 3% polyvidone alcoholic solution system soft material, cross 18 mesh sieve system granules with 46g microcrystalline Cellulose mix homogeneously, 60 ℃ of dryings 30 minutes, granulate, adding 4g Pulvis Talci, mixing, tabletting, promptly.
Embodiment seven (FUFANG DANSHEN DIWAN Radix Notoginseng component finger printing test example)
1, instrument and reagent
Instrument: adopt Agilent 1100 liquid chromatograph, comprise quaternary pump, online degasser, automatic sampler, DAD detector, column oven, Chemstation work station; BS210S electronic balance (1/10
-4G) (Beijing Sai Duolisi company), METTLERAE240 electronic balance (1/10
-4G or 1/10
-5G) (prunus mume (sieb.) sieb.et zucc. Teller-Tuo benefit (Shanghai) Co., Ltd.), LD4-2 centrifuge (4000r/min) (Beijing Medical Centrifugal Machine Factory), digital display thermostat water bath (the long wind company limited in Tianjin), 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 filter (HENGGAO T﹠amp; D), synthetic fibers filter membrane (aperture 0.45 μ m) (going up Haixing County inferior scavenging material factory); C
18(filler is C to pillar
18H
17The liquid chromatograph immobile phase, 50～100 orders, chemical reagent two factories in Tianjin produce.Dry column-packing 600mg, column internal diameter 1cm).
Reagent: acetonitrile (chromatographically pure, U.S. Merck company), acetic acid (top grade is pure), WAHAHA pure water.
2, the preparation of FUFANG DANSHEN DIWAN control sample
The preparation of FUFANG DANSHEN DIWAN test sample: take by weighing each batch FUFANG DANSHEN DIWAN 1.0g among the embodiment one, be dissolved in 10ml 4% ammonia, ultrasonic dissolution, cross 0.45 μ m filter membrane, get 5ml filtrate and cross C-18 pillar (500mg filler), the methanol aqueous ammonia eluting of 20ml 20% is collected meoh eluate in the 5ml volumetric flask, standardize solution, centrifugal standby; Parallel 2 parts, sample size 20 μ l.
The preparation of FUFANG DANSHEN DIWAN intermediate test sample: take by weighing each batch Salvia miltiorrhiza and Panax notoginseng extractum 0.2g among the embodiment one, be dissolved in 10ml 4% ammonia, ultrasonic dissolution, cross 0.45 μ m filter membrane, get 5ml filtrate and cross the C-18 pillar, elder generation washes with the ammonia spirit of the methanol 4% of 15ml 20%, reuse 20ml washing, collect meoh eluate in the 5ml volumetric flask, standardize solution, centrifugal standby.Parallel 2 parts, sample size 20 μ l.
The preparation of pseudo-ginseng test sample: take by weighing medical material 2.5g in Backflow bottle, add distilled water 50ml, refluxed 1.5 hours, filter, add the 50ml distilled water in the filtering residue, refluxed 1 hour, merging filtrate is dissolved in the 100ml measuring bottle surely, and centrifugal filtration is standby.Parallel 2 parts, sample size 10 μ l.
3, HPLC analysis condition
Agilent SB-C
18Analytical column (4.6mm * 250mm, Zorbax SB USCL010304); Mobile phase: A is 0.01% (V/V) glacial acetic acid aqueous solution mutually, and B is mutually for containing the acetonitrile solution of 0.01% glacial acetic acid.Flow velocity 0.8mlmin
-1Detect wavelength 203nm; 30 ℃ of column temperatures.
Gradient elution program such as following table:
| ????Time | ??A：0.01％HAC-H2O(％)(v/v) | ??B：0.01％HAC-CH3CN(％)(v/v) |
| ????0 ????15 ????25 ????40 ????50 ????65 ????75 | ????80 ????65 ????65 ????57 ????57 ????42 ????25 | ????20 ????35 ????35 ????43 ????43 ????58 ????75 |
FUFANG DANSHEN DIWAN Radix Notoginseng finger printing composition title:
| Peak 1- | Peak 2- | Peak 3- | Peak 4- | Peak 5- | Peak 6- | Peak 7- |
| Panax Notoginseng saponin R 1 | Ginsenoside R e+R g1 | Ginsenoside R b1 | Panax Notoginseng saponin R 2 | Ginsenoside R h1 | Ginsenoside Rh liso. (F1) | Ginsenoside R d |
| Peak 8- | Peak 9- | Peak 10- | Peak 11- | Peak 12- | Peak 13- | Peak 14- |
| Panax Notoginseng saponin R 2-H2O | Panax Notoginseng saponin R 2-H2O | Ginsenoside R g6/F 4 | Ginsenoside R k3/R h4(R k3) | Ginsenoside R k3/R h4(R h4) | Ginsenoside R k1/R g5(R k1) | Ginsenoside R k1/R g5(R g5) |
Amount to reply side's Radix Salviae Miltiorrhizae extractum surplus 200 is carried out Radix Salviae Miltiorrhizae, Radix Notoginseng fingerprint map analyzing respectively, its similarity is all more than 90%.Now gather the retention time of collection of illustrative plates, the meansigma methods and the RSD value of peak area as follows:
Radix Notoginseng finger printing part
| Peak number | Average retention time | The RSD% of retention time | Average peak area | The RSD% of peak area | The unimodal percentage ratio that accounts for total peak area |
| ????1 | ????10.85 | ????0.08 | ??557.29 | ????15.67 | ????5.36％ |
| ????2 | ????12.1 | ????0.06 | ??2728.83 | ????16.66 | ????26.23％ |
| ????3 | ????20.33 | ????0.08 | ??3704.31 | ????14.15 | ????35.61％ |
| ????4 | ????20.86 | ????0.07 | ??272.69 | ????12.54 | ????2.62％ |
| ????5 | ????23.28 | ????0.08 | ??369.12 | ????21.52 | ????3.55％ |
| ????6 | ????24.48 | ????0.08 | ??190.23 | ????17.45 | ????1.83％ |
| ????7 | ????28.82 | ????1.36 | ??289.16 | ????17.71 | ????2.78％ |
| ????8 | ????42.93 | ????0.07 | ??239.14 | ????18.84 | ????2.30％ |
| ????9 | ????45.66 | ????0.06 | ??445.17 | ????19.56 | ????4.28％ |
| ????10 | ????47.85 | ????0.06 | ??723.59 | ????14.24 | ????6.96％ |
| ????11 | ????68.17 | ????0.03 | ??407.66 | ????10.86 | ????3.92％ |
| ????12 | ????69.4 | ????0.03 | ??476.31 | ????15.46 | ????4.58％ |
Amount to reply side's Radix Salviae Miltiorrhizae drop pill surplus 200 is carried out Radix Salviae Miltiorrhizae, Radix Notoginseng fingerprint map analyzing respectively, its similarity is all more than 90%.Now gather the retention time of collection of illustrative plates, the meansigma methods and the RSD value of peak area as follows:
Radix Notoginseng finger printing part
| Peak number | Average retention time | Retention time RSD% | Average peak area | Peak area RSD% | The unimodal percentage ratio that accounts for total peak area |
| ????1 | ????10.87 | ????0.45 | ??506.92 | ????13.03 | ????4.27％ |
| ????2 | ????12.12 | ????0.34 | ??2723.73 | ????12.11 | ????22.93％ |
| ????3 | ????20.34 | ????0.23 | ??1684.49 | ????18.95 | ????14.18％ |
| ????4 | ????20.86 | ????0.16 | ??231.84 | ????18.99 | ????1.95％ |
| ????5 | ????23.29 | ????0.25 | ??565.78 | ????13.8 | ????4.76％ |
| ????6 | ????24.48 | ????0.28 | ??309.39 | ????18.98 | ????2.60％ |
| ????7 | ????29 | ????0.62 | ??345.32 | ????14.28 | ????2.91％ |
| ????8 | ????41.21 | ????0.25 | ??436.06 | ????10.88 | ????3.67％ |
| ????9 | ????42.94 | ????0.21 | ??665.38 | ????11.82 | ????5.60％ |
| ????10 | ????44.16 | ????0.21 | ??472.84 | ????14.59 | ????3.98％ |
| ????11 | ????45.68 | ????0.23 | ??947.39 | ????16.06 | ????7.97％ |
| ????12 | ????47.88 | ????0.25 | ??1547.8 | ????13.25 | ????13.03％ |
| ????13 | ????68.21 | ????0.13 | ??622.91 | ????10.39 | ????5.24％ |
| ????14 | ????69.43 | ????0.12 | ??820.24 | ????12.93 | ????6.90％ |
Embodiment eight (foundation of FUFANG DANSHEN DIWAN reference fingerprint)
1, instrument and reagent
Instrument: adopt Agilent 1100 liquid chromatograph, comprise quaternary pump, online degasser, automatic sampler, DAD detector, column oven, Chemstation work station; BS210S electronic balance (1/10
-4G) (Beijing Sai Duolisi company), METTLERAE240 electronic balance (1/10
-4G or 1/10
-5G) (prunus mume (sieb.) sieb.et zucc. Teller-Tuo benefit (Shanghai) Co., Ltd.), LD4-2 centrifuge (4000r/min) (Beijing Medical Centrifugal Machine Factory), digital display thermostat water bath (the long wind company limited in Tianjin), 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 filter (HENGGAO T﹠amp; D), synthetic fibers filter membrane (aperture 0.45 μ m) (going up Haixing County inferior scavenging material factory); C
18(filler is C to pillar
18H
17The liquid chromatograph immobile phase, 50～100 orders, chemical reagent two factories in Tianjin produce.Dry column-packing 600mg, column internal diameter 1cm).
Reagent: acetonitrile (chromatographically pure, U.S. Merck company), acetic acid (top grade is pure), WAHAHA pure water.
2, test sample preparation
Claim FUFANG DANSHEN DIWAN 1.0g, be dissolved in 10mL 4% ammonia, ultrasonic dissolution, cross 0.45 μ m filter membrane, get the C-18 pillar that 5mL filtrate is crossed the 500mg filler, the methanol 4% ammonia spirit flushing of 20mL 20%, abandon flushing liquor, water lotion is abandoned in reuse 20ml washing, the reuse methanol-eluted fractions, collect meoh eluate in the 5mL volumetric flask, standardize solution, centrifugal standby, parallel 2 parts, sample size 20 μ L;
The preparation of FUFANG DANSHEN DIWAN intermediate test sample: take by weighing each batch Salvia miltiorrhiza and Panax notoginseng extractum 0.2g among the embodiment two, be dissolved in 10mL 4% ammonia, ultrasonic dissolution, cross 0.45 μ m filter membrane, get the C-18 pillar that 5mL filtrate is crossed the 500mg filler, the methanol 4% ammonia spirit flushing of 20mL 20%, abandon flushing liquor, water lotion is abandoned in reuse 20ml washing, reuse methanol Shen is taken off, collect meoh eluate in the 5mL volumetric flask, standardize solution, centrifugal standby, parallel 2 parts, sample size 20 μ L;
The preparation of pseudo-ginseng test sample: take by weighing medical material 2.5g in Backflow bottle, add distilled water 50ml, refluxed 1.5 hours, filter, add the 50ml distilled water in the filtering residue, refluxed 1 hour, merging filtrate is dissolved in the 100ml measuring bottle surely, and centrifugal filtration is standby.Parallel 2 parts, sample size 10 μ l.
3, HPLC analysis condition
Agilent SB-C
18Analytical column (4.6mm * 250mm, Zorbax SB USCL010304); Mobile phase: A is 0.01% (V/V) glacial acetic acid aqueous solution mutually, and B is mutually for containing the acetonitrile solution of 0.01% glacial acetic acid.Flow velocity 0.8mlmin
-1Detect wavelength 203nm; 30 ℃ of column temperatures.
Gradient elution program such as following table:
| ????Time | ??A：0.01％HAC-H2O(％) | ??B：0.01％HAC-CH3CN(％) |
| ????0 ????15 ????25 ????40 ????50 ????65 ????75 | ????80 ????65 ????65 ????57 ????57 ????42 ????25 | ????20 ????35 ????35 ????43 ????43 ????58 ????75 |
In the described finger printing, Radix Notoginseng component chemical composition absworption peak has 14 in the FUFANG DANSHEN DIWAN, and the absworption peak that wherein unimodal area surpasses total peak area 2% has 13, is respectively:
No. 1 peak, average retention time RT is 10.87min, and RSD is 0.31%, and peak area is 506.92, and RSD is 13.03%;
No. 2 peaks, average retention time RT is 12.12min, and RSD is 0.34%, and peak area is 2723.73, and RSD is 12.11%;
No. 3 peaks, average retention time RT is 20.34min, and RSD is 0.23%, and peak area is 1684.49, and RSD is 18.59%;
No. 5 peaks, average retention time RT is 23.29min, and RSD is 0.25%, and peak area is 565.78, and RSD is 13.80%;
No. 6 peaks, average retention time RT is 24.48min, and RSD is 0.28%, and peak area is 309.39, and RSD is 18.98%;
No. 7 peaks, average retention time RT is 29.00min, and RSD is 0.62%, and peak area is 345.32, and RSD is 14.28%;
No. 8 peaks, average retention time RT is 41.21min, and RSD is 0.25%, and peak area is 436.06, and RSD is 10.88%;
No. 9 peaks, average retention time RT is 42.94min, and RSD is 0.21%, and peak area is 665.38, and RSD is 11.82%;
No. 10 peaks, average retention time RT is 44.16min, and RSD is 0.21%, and peak area is 472.84, and RSD is 14.59%;
No. 11 peaks, average retention time RT is 45.68min, and RSD is 0.23%, and peak area is 947.39, and RSD is 16.06%;
No. 12 peaks, average retention time RT is 47.88min, and RSD is 0.25%, and peak area is 1547.80, and RSD is 13.25%;
No. 13 peaks, average retention time RT is 68.21min, and RSD is 0.13%, and peak area is 622.91, and RSD is 10.39%;
No. 14 peaks, average retention time RT is 69.43min, and RSD is 0.12%, and peak area is 820.24, and RSD is 12.94%;
In the described finger printing, the component chemical composition absworption peak of pseudo-ginseng test sample has 5, and the absworption peak that wherein unimodal area surpasses total peak area 2% has 5, is respectively:
No. 1 peak, average retention time RT is 10.81min, and RSD is 0.06%, and peak area is 539.57, and RSD is 17.73%;
No. 2 peaks, average retention time RT is 12.03min, and RSD is 0.02%, and peak area is 2482.50, and RSD is 8.74%;
No. 3 peaks, average retention time RT is 20.16min, and RSD is 0.11%, and peak area is 1514.5, and RSD is 12.02%;
No. 4 the average retention time RT in peak is 23.04min, and RSD is 0.07%, and peak area is 250.63, and RSD is 18.25%;
No. 5 peaks, average retention time RT is 28.42min, and RSD is 0.27%, and peak area is 356.20, and RSD is 15.30%;
Radix Notoginseng component chemical composition absworption peak has 12 in the FUFANG DANSHEN DIWAN intermediate, and the absworption peak that wherein unimodal area surpasses total peak area 2% has 11, is respectively:
No. 1 peak, average retention time RT is 10.85min, and RSD is 0.08%, and peak area is 557.29, and RSD is 15.67%;
No. 2 peaks, average retention time RT is 12.10min, and RSD is 0.06%, and peak area is 2728.83, and RSD is 16.66%;
No. 3 peaks, average retention time RT is 20.33min, and RSD is 0.08%, and peak area is 3704.31, and RSD is 14.15%;
No. 4 peaks, average retention time RT is 23.86min, and RSD is 0.07%, and peak area is 272.69, and RSD is 12.54%;
No. 5 peaks, average retention time RT is 23.28min, and RSD is 0.08%, and peak area is 369.12, and RSD is 21.52%;
No. 7 peaks, average retention time RT is 28.82min, and RSD is 1.36%, and peak area is 289.16, and RSD is 17.71%;
No. 8 peaks, average retention time RT is 42.93min, and RSD is 0.07%, and peak area is 239.14, and RSD is 18.84%;
No. 9 peaks, average retention time RT is 45.66min, and RSD is 0.06%, and peak area is 445.17, and RSD is 19.56%;
No. 10 peaks, average retention time RT is 47.85min, and RSD is 0.06%, and peak area is 723.59, and RSD is 14.24%;
No. 11 peaks, average retention time RT is 68.17min, and RSD is 0.03%, and peak area is 407.66, and RSD is 10.86%;
No. 12 peaks, average retention time RT is 69.4min, and RSD is 0.03%, and peak area is 476.31, and RSD is 15.46%.
Claims (11)
1. the method for quality control of a FUFANG DANSHEN DIWAN is characterized in that comprising the steps:
(a). the foundation of FUFANG DANSHEN DIWAN reference fingerprint
The preparation of FUFANG DANSHEN DIWAN control sample solution:
Claim FUFANG DANSHEN DIWAN, be dissolved in the ammonia of 1～20mL1～8% ultrasonic dissolution, cross 0.30～0.60 μ m filter membrane, get the C-18 pillar that 2～10mL filtrate is crossed filler, flushing liquor is abandoned in methanol 1～8% ammonia spirit flushing of 5～40mL8～35%, reuse 5～35ml washing, abandon water lotion, the reuse methanol-eluted fractions is collected meoh eluate in 1～15mL volumetric flask, standardize solution, centrifugal standby;
The mensuration of FUFANG DANSHEN DIWAN reference fingerprint:
Draw above-mentioned control sample solution and inject chromatograph of liquid, use high performance liquid chromatography to measure, obtain the FUFANG DANSHEN DIWAN reference fingerprint, chromatographic condition: chromatographic column is that octadecylsilane chemically bonded silica is a filler; Adopt gradient elution, mobile phase A is a glacial acetic acid aqueous solution, and Mobile phase B is the glacial acetic acid acetonitrile solution; Detect wavelength 200～210nm;
(b). the mensuration of FUFANG DANSHEN DIWAN product fingerprint collection of illustrative plates to be measured:
Get FUFANG DANSHEN DIWAN product to be measured, measure the finger printing of this product to be measured according to Step By Condition described in above-mentioned (a);
(c). described FUFANG DANSHEN DIWAN product fingerprint collection of illustrative plates to be measured and described FUFANG DANSHEN DIWAN reference fingerprint are compared, discern the quantity of its absworption peak, to determine whether product quality is qualified.
2. the method for quality control of FUFANG DANSHEN DIWAN as claimed in claim 1 is characterized in that:
The preparation method of FUFANG DANSHEN DIWAN control sample solution is in described (a) step, claims FUFANG DANSHEN DIWAN, is dissolved in 5～15mL2～6% ammonia, ultrasonic dissolution is crossed 0.35～0.55 μ m filter membrane, gets the C-18 pillar that 2～10mL filtrate is crossed filler, methanol 2～6% ammonia spirits flushing of 10～30mL10～30%, abandon flushing liquor, water lotion is abandoned in reuse 10～30ml washing, the reuse methanol-eluted fractions, collect meoh eluate in 1～10mL volumetric flask, standardize solution, centrifugal standby;
Chromatographic condition: chromatographic column is that octadecylsilane chemically bonded silica is a filler; Adopt gradient elution, mobile phase A is 0.01% glacial acetic acid aqueous solution mutually, and Mobile phase B is mutually for containing the acetonitrile solution of 0.01% glacial acetic acid; The gradient elution program is as follows:
In the time of 0 minute, mobile phase A is that 80% 0.01% glacial acetic acid aqueous solution, Mobile phase B are the acetonitrile solution of 20% 0.01% glacial acetic acid;
In the time of 15 minutes, mobile phase A is that 65% 0.01% glacial acetic acid aqueous solution, Mobile phase B are the acetonitrile solution of 35% 0.01% glacial acetic acid;
In the time of 25 minutes, mobile phase A is that 65% 0.01% glacial acetic acid aqueous solution, Mobile phase B are the acetonitrile solution of 35% 0.01% glacial acetic acid;
In the time of 40 minutes, mobile phase A is that 57% 0.01% glacial acetic acid aqueous solution, Mobile phase B are the acetonitrile solution of 43% 0.01% glacial acetic acid;
In the time of 50 minutes, mobile phase A is that 57% 0.01% glacial acetic acid aqueous solution, Mobile phase B are the acetonitrile solution of 43% 0.01% glacial acetic acid;
In the time of 65 minutes, mobile phase A is that 42% 0.01% glacial acetic acid aqueous solution, Mobile phase B are the acetonitrile solution of 58% 0.01% glacial acetic acid;
In the time of 75 minutes, mobile phase A is that 25% 0.01% glacial acetic acid aqueous solution, Mobile phase B are the acetonitrile solution of 75% 0.01% glacial acetic acid;
Sample size 5～45 μ L; Flow velocity 0.8mLmin-1; Detect wavelength 201～205nm; 25～35 ℃ of column temperatures.
3. the method for quality control of FUFANG DANSHEN DIWAN as claimed in claim 2 is characterized in that:
The preparation method of FUFANG DANSHEN DIWAN control sample solution is in described (a) step, claims FUFANG DANSHEN DIWAN 0.4～1.5g, is dissolved in 10mL4% ammonia, ultrasonic dissolution is crossed 0.45 μ m filter membrane, gets the C-18 pillar that 5mL filtrate is crossed the 500mg filler, flushing liquor is abandoned in the methanol 4% ammonia spirit flushing of 20mL20%, reuse 20ml washing, abandon water lotion, the reuse methanol-eluted fractions is collected meoh eluate in 5mL volumetric flask, standardize solution, centrifugal standby, sample size 20 μ L;
Chromatographic condition: sample size 20 μ L; Flow velocity 0.8mLmin
-1Detect wavelength 203nm; 30 ℃ of column temperatures.
4. as claim 1 or 2 or 3 described quality control of compound Danshen root drops, it is characterized in that contrasting in the foundation of fingerprint pattern of compound salvia dropping pills, the configuration proportion of its mobile phase A solution is to prepare by volume, and the configuration proportion of Mobile phase B solution is to prepare by volume.
5. as the product quality control method of claim 1,2 or 3 described FUFANG DANSHEN DIWAN, it is characterized in that, 14 absworption peaks are arranged in the reference fingerprint of described FUFANG DANSHEN DIWAN, and the absworption peak that wherein unimodal area surpasses total peak area 10% has 3, is respectively:
No. 2 peaks, average retention time RT is 12.12min, and RSD is 0.34%, and peak area is 2723.73, and RSD is 12.11%;
No. 3 peaks, average retention time RT is 20.34min, and RSD is 0.23%, and peak area is 1684.49, and RSD is 18.59%;
No. 12 peaks, average retention time RT is 47.88min, and RSD is 0.25%, and peak area is 1547.80, and RSD is 13.25%.
6. as claim 1,2 or 3 described FUFANG DANSHEN DIWAN product quality control methods, it is characterized in that in the reference fingerprint of described FUFANG DANSHEN DIWAN 14 absworption peaks being arranged, the absworption peak that wherein unimodal area surpasses total peak area 5% has 7, is respectively:
No. 2 peaks, average retention time RT is 12.12min, and RSD is 0.34%, and peak area is 2723.73, and RSD is 12.11%;
No. 3 peaks, average retention time RT is 20.34min, and RSD is 0.23%, and peak area is 1684.49, and RSD is 18.59%;
No. 9 peaks, average retention time RT is 42.94min, and RSD is 0.21%, and peak area is 665.38, and RSD is 11.82%;
No. 11 peaks, average retention time RT is 45.68min, and RSD is 0.23%, and peak area is 947.39, and RSD is 16.06%;
No. 12 peaks, average retention time RT is 47.88min, and RSD is 0.25%, and peak area is 1547.80, and RSD is 13.25%;
No. 13 peaks, average retention time RT is 68.21min, and RSD is 0.13%, and peak area is 622.91, and RSD is 10.39%;
No. 14 peaks, average retention time RT is 69.43min, and RSD is 0.12%, and peak area is 820.24, and RSD is 12.94%.7. as the product quality control method of claim 1,2 or 3 described FUFANG DANSHEN DIWAN, it is characterized in that, 8 absworption peaks are arranged in the reference fingerprint of described FUFANG DANSHEN DIWAN, and its unimodal area all has 13 above 2% absworption peak of total peak area, is respectively:
No. 1 peak, average retention time RT is 10.87min, and RSD is 0.31%, and peak area is 506.92, and RSD is 13.03%;
No. 2 peaks, average retention time RT is 12.12min, and RSD is 0.34%, and peak area is 2723.73, and RSD is 12.11%;
No. 3 peaks, average retention time RT is 20.34min, and RSD is 0.23%, and peak area is 1684.49, and RSD is 18.59%;
No. 5 peaks, average retention time RT is 23.29min, and RSD is 0.25%, and peak area is 565.78, and RSD is 13.80%;
No. 6 peaks, average retention time RT is 24.48min, and RSD is 0.28%, and peak area is 309.39, and RSD is 18.98%;
No. 7 peaks, average retention time RT is 29.00min, and RSD is 0.62%, and peak area is 345.32, and RSD is 14.28%;
No. 8 peaks, average retention time RT is 41.21min, and RSD is 0.25%, and peak area is 436.06, and RSD is 10.88%;
No. 9 peaks, average retention time RT is 42.94min, and RSD is 0.21%, and peak area is 665.38, and RSD is 11.82%;
No. 10 peaks, average retention time RT is 44.16min, and RSD is 0.21%, and peak area is 472.84, and RSD is 14.59%;
No. 11 peaks, average retention time RT is 45.68min, and RSD is 0.23%, and peak area is 947.39, and RSD is 16.06%;
No. 12 peaks, average retention time RT is 47.88min, and RSD is 0.25%, and peak area is 1547.80, and RSD is 13.25%;
No. 13 peaks, average retention time RT is 68.21min, and RSD is 0.13%, and peak area is 622.91, and RSD is 10.39%;
No. 14 peaks, average retention time RT is 69.43min, and RSD is 0.12%, and peak area is 820.24, and RSD is 12.94%.
8. as claim 1,2 or 3 described quality control of compound Danshen root drops, it is characterized in that, described FUFANG DANSHEN DIWAN product fingerprint collection of illustrative plates to be measured and described FUFANG DANSHEN DIWAN reference fingerprint are relatively, when the two finger printing has absworption peak identical more than 3 or 3, think the up-to-standard of described FUFANG DANSHEN DIWAN product to be measured.
9. the method for quality control of FUFANG DANSHEN DIWAN as claimed in claim 8, it is characterized in that, described FUFANG DANSHEN DIWAN product fingerprint collection of illustrative plates to be measured and described FUFANG DANSHEN DIWAN reference fingerprint are relatively, when the two finger printing has absworption peak identical more than 5 or 5, think the up-to-standard of described FUFANG DANSHEN DIWAN product to be measured.
10. the method for quality control of FUFANG DANSHEN DIWAN as claimed in claim 8, it is characterized in that, described FUFANG DANSHEN DIWAN product fingerprint collection of illustrative plates to be measured and described FUFANG DANSHEN DIWAN reference fingerprint are relatively, when the two finger printing has absworption peak identical more than 7 or 7, think the up-to-standard of described FUFANG DANSHEN DIWAN product to be measured.
11. quality control of compound Danshen root drops as claimed in claim 8, it is characterized in that tested FUFANG DANSHEN DIWAN product fingerprint collection of illustrative plates and contrast fingerprint pattern of compound salvia dropping pills compare, when the two finger printing has absworption peak identical more than 13 or 13, think the up-to-standard of described FUFANG DANSHEN DIWAN product to be measured.
12, quality control of compound Danshen root drops as claimed in claim 8, it is characterized in that tested FUFANG DANSHEN DIWAN product fingerprint collection of illustrative plates and contrast fingerprint pattern of compound salvia dropping pills compare, the total peak of the two finger printing reaches 14, thinks that just FUFANG DANSHEN DIWAN product to be measured is qualified products.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100442049C (en) * | 2004-03-17 | 2008-12-10 | 天津天士力制药股份有限公司 | Method for measuring fingerprint pattern of compound salvia dropping pills |
| CN108333282A (en) * | 2018-04-24 | 2018-07-27 | 山东农业大学 | A kind of method of a variety of phenolic acid class and tanshinone component in Rapid Simultaneous Determination Fufang Danshen Pian |
| CN109196354A (en) * | 2016-05-30 | 2019-01-11 | 株式会社岛津制作所 | Chromatogram arrangement |
| CN111487350A (en) * | 2020-05-18 | 2020-08-04 | 陕西中医药大学 | Quality detection method of salvia miltiorrhiza-panax notoginseng medicine pair |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1472532A (en) * | 2002-08-02 | 2004-02-04 | 上海蔡同德堂中药制药厂 | Method for determining salviolic acid beta content in red sage root |
| CN100412545C (en) * | 2002-12-23 | 2008-08-20 | 北京采瑞医药有限公司 | Method for controlling quality of compound red sage root preparation used for treating cardio-cerebral vascualr disease |
-
2005
- 2005-03-16 CN CNB2005100546967A patent/CN100381813C/en active Active
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100442049C (en) * | 2004-03-17 | 2008-12-10 | 天津天士力制药股份有限公司 | Method for measuring fingerprint pattern of compound salvia dropping pills |
| CN109196354A (en) * | 2016-05-30 | 2019-01-11 | 株式会社岛津制作所 | Chromatogram arrangement |
| CN108333282A (en) * | 2018-04-24 | 2018-07-27 | 山东农业大学 | A kind of method of a variety of phenolic acid class and tanshinone component in Rapid Simultaneous Determination Fufang Danshen Pian |
| CN111487350A (en) * | 2020-05-18 | 2020-08-04 | 陕西中医药大学 | Quality detection method of salvia miltiorrhiza-panax notoginseng medicine pair |
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