CN101156894B - Detection method of apricot red injection - Google Patents
Detection method of apricot red injection Download PDFInfo
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- CN101156894B CN101156894B CN2007102018851A CN200710201885A CN101156894B CN 101156894 B CN101156894 B CN 101156894B CN 2007102018851 A CN2007102018851 A CN 2007102018851A CN 200710201885 A CN200710201885 A CN 200710201885A CN 101156894 B CN101156894 B CN 101156894B
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Abstract
The invention provides a quality control method for Xingdan injection. The method comprises a finger print test of the Xingdan injection; differentiation tests of components of gingko leaf medicine, gingko leaf extractive, gingko leaf total flavone glycoside, and gingko leaf total terpene lactone, etc.; content tests of components of Danshensu, protocatechuic aldehyde, salvianolic acid B or the magnesium salt thereof, tanshinone IIA, quercetin, kaempferide, etc.; compared with the prior art, the quality control method of the invention is more effective in controlling the quality of the Chinese medicine injection products produced with the gingko leaves, the red sage roots and the extractive thereof, with high accuracy and high stability.
Description
The present patent application is the dividing an application of " method of quality control of Xingdan injection " of submit applications on January 24th, 2006102000711,2006.Requirement is priority date with it in 200510003011.6 applyings date of CN of submitting on February 7th, 2005.
Technical field
The present invention is a kind of method of quality control of Xingdan injection, belongs to technical field of Chinese medicine.
Background technology
Cardiovascular and cerebrovascular disease such as coronary heart disease, cerebral thrombosis, hypertension, cerebral infarction etc. all are one of the most common and diseases that harm is maximum in the world today, also are commonly encountered diseases, the frequently-occurring disease of harm China people ' s health, have become human mortality's one of the main reasons; It was reported that sickness rate in recent years has and increases trend year by year, and in, young patient constantly increases.In order to reach the purpose of control, the Qiyuanyide Medicines Inst., Beijing had once submitted a number of patent application and had been " 200410022288.9 ", name is called the application of " a kind of Chinese medicine preparation for the treatment of cardiovascular and cerebrovascular disease and preparation method thereof ", it is made by Radix Salviae Miltiorrhizae and Folium Ginkgo, the ejection preparation of preparation can play and improve cardiac muscle and brain tissue metabolism, increase coronary artery and brain vessel blood, improve the effect of blood confessions such as cardiac muscle and cerebral tissue, for treatment cardiovascular and cerebrovascular disease such as coronary heart disease, angina pectoris, arrhythmia, cerebral thrombosis, alzheimer disease etc. have curative effect preferably, simultaneously can human body immunity improving power, resist the disease takes place; But pharmaceutical preparation must be on the basis that guarantees the constant product quality controllable safety, the more new development that could not lack, in order better to control the quality of said preparation, guarantee the safety of medication, better instruct and produce, make technology controlling and process rationally strict more, make consumer's energy full appreciation product quality, need research, control this injection method for quality.
Summary of the invention
The objective of the invention is to: the method for quality control that a kind of Xingdan injection is provided, this method at following product to the means of relevant production, index that testing agency provides detection, detection, technical method etc., so that better control the quality of said preparation, guarantee the safety of medication, can better instruct production, make controlling of production process strict more rationally, make the consumer can full appreciation product quality, at product be:
1) by Folium Ginkgo medical material: red rooted salvia=20-80: the 80-20 prescription, difference or merging adopt water or alcoholic solution to extract, carry out suitably refining, mixing with in the sedimentation method, column chromatography, solvent extraction and the supercritical extraction one or more then, make injection then, comprise the injection that is directly used in drug administration by injection, need to be used for after the dilution concentrated solution for injection of intravenous drip, directly for the glucose intravenous infusion of intravenous drip and sodium chloride intravenous infusion and the injectable sterile powder and the aseptic block that make with freeze-drying or spray drying method;
2) by Folium Ginkgo extract: Radix Salviae Miltiorrhizae extract=20-80: the injection that the 80-20 prescription is made, comprise the injection that is directly used in drug administration by injection, the concentrated solution for injection that is used for intravenous drip after needing to dilute, the glucose intravenous infusion of direct confession intravenous drip and sodium chloride intravenous infusion and the injectable sterile powder and the aseptic block that make with freeze-drying or spray drying method, described extract can derive from commercially available, also can adopt water or alcoholic solution to extract, use the sedimentation method then, column chromatography, in solvent extraction and the supercritical extraction one or more carry out suitably refining obtaining afterwards.
Or number of patent application is: 200410022288.9, and name is called: the ejection preparation of the preparation method preparation that " a kind of Chinese medicine for the treatment of cardiovascular and cerebrovascular disease and preparation method thereof " provides.
The present invention constitutes like this:
The method of quality control of Xingdan injection comprises following all or part of content:
The test of the finger printing of Xingdan injection comprises with Radix Salviae Miltiorrhizae and Folium Ginkgo flavone constituents being characterized as main finger printing and based in the finger printing of Folium Ginkgo terpene lactone composition characteristics one or both.
Wherein, fingerprint atlas detection method comprises following one or both:
A, the test of employing liquid chromatography are characterized as main finger printing with Radix Salviae Miltiorrhizae and Folium Ginkgo flavone constituents:
(1) preparation of need testing solution: it is an amount of to get the red ejection preparation of Fructus Pruni to be measured, adds water or methanol or dissolve with ethanol or dilution, shakes up, and filters, and gets subsequent filtrate as need testing solution;
(2) preparation of object of reference solution: get the main active reference substance in an amount of Radix Salviae Miltiorrhizae and the Folium Ginkgo medical material, comprise a kind of in danshensu sodium, protocatechualdehyde, salvianolic acid B or its magnesium salt, Quercetin, kaempferide, the isorhamnetin, water or methanol or dissolve with ethanol, be settled to suitable concn, as object of reference solution;
(3) chromatographic condition: the chromatographic column adopting octadecylsilane chemically bonded silica is a filler: mobile phase is acetonitrile or methanol-0.01mol/L～2mol/L biphosphate sodium water solution or 0.01mol/L～2mol/L potassium dihydrogen phosphate aqueous solution or 0.01mol/L～2mol/L sodium hydrogen phosphate aqueous solution or water or 0.1%～5% glacial acetic acid solution or 0.1%～5% formic acid solution or 0.02%～5% phosphoric acid solution, gradient elution, flow velocity is 0.5～2.0ml/min, one or several or the evaporation photodetector that detect wavelength and be in 190～410nm scope detect, and column temperature is in 20～60 ℃ of scopes;
(4) formulation of standard finger-print: the means of testing that is characterized as main finger printing with said method as formulation with Radix Salviae Miltiorrhizae and Folium Ginkgo flavone constituents; According to 10 batches or 10 batches of collection of illustrative plates that above test sample is measured, formulating standard finger-print, is benchmark with the retention time of the object of reference chromatographic peak determined, calculates the relative retention time of other total chromatographic peak, in the described standard finger-print, total peak has 3～50;
(5) with the described method in (1)～(3) as the means of testing that is characterized as main finger printing in the Xingdan injection to be measured with Radix Salviae Miltiorrhizae and Folium Ginkgo flavone constituents, the preparation testing sample finger printing;
(6) with the finger printing of Xingdan injection to be measured and the contrast of above-mentioned standard finger-print, in should meeting the following requirements partly or entirely:
I. calculate the similarity of the finger printing and the standard finger-print of Xingdan injection to be measured, should be 0.80～1.00;
II. in the Xingdan injection finger printing to be measured, non-total peak area must not surpass 10% of total peak area;
The odds ratio that each total peak area in the ratio of 5%～60% total peak area and the standard finger-print arranged in the Xingdan injection finger printing III. to be measured, its difference must not be greater than ± 50%;
B, employing liquid chromatography are tested the finger printing based on Folium Ginkgo terpene lactone composition characteristics:
(1) preparation of need testing solution: it is an amount of to get the red ejection preparation of Fructus Pruni to be measured, be dissolved in water, add 0.2%～30% hydrochloric acid solution, with ethyl acetate or n-butyl alcohol or chloroform or dichloromethane extraction, combining extraction liquid, wash with 0.5%～20% sodium acetate solution, divide and get sodium acetate liquid,, merge ethyl acetate or n-butyl alcohol or chloroform or dichloromethane extract and washing liquid with ethyl acetate or n-butyl alcohol or chloroform or washed with dichloromethane, wash with water, merge water lotion,, merge ethyl acetate or n-butyl alcohol or chloroform or dichloromethane solution with ethyl acetate or n-butyl alcohol or chloroform or washed with dichloromethane, reclaim ethyl acetate or n-butyl alcohol or chloroform or dichloromethane to doing, residue adds acetone or methanol or ethanol makes dissolving, shakes up, and filters, filter, get subsequent filtrate as need testing solution;
(2) preparation of object of reference solution: get a kind of in bilobalide or ginkalide A or ginkalide B or the ginkalide C, with methanol or dissolve with ethanol, be settled to suitable concn, as object of reference solution;
95～5) or methanol or methanol-oxolane (5～95: 95～5) (3) chromatographic condition: the chromatographic column adopting octadecylsilane chemically bonded silica is a filler: mobile phase A is acetonitrile or acetonitrile-oxolane (5～95:, Mobile phase B is water or 0.1%～5% glacial acetic acid or 0.1%～5% formic acid or 0.005%～5% phosphoric acid solution, gradient elution, flow velocity is 0.5～2.0ml/min, detect wavelength is that one or several or evaporative light scattering detector in 190～410nm scope detects, and column temperature is in 20～60 ℃ of scopes;
(4) formulation of standard finger-print: the means of testing that is characterized as main finger printing with said method as formulation with Folium Ginkgo terpene lactone constituents; According to 10 batches or 10 batches of collection of illustrative plates that above test sample is measured, formulating standard finger-print, is benchmark with the retention time of the object of reference chromatographic peak determined, calculates the relative retention time of other total chromatographic peak, in the described standard finger-print, total peak has 3～30;
(5) with the described method in (1)～(3) as the means of testing that is characterized as main finger printing in the Xingdan injection to be measured with Folium Ginkgo terpene lactone constituents, the preparation testing sample finger printing;
(6) with the finger printing of Xingdan injection to be measured and the contrast of above-mentioned standard finger-print, in should meeting the following requirements partly or entirely:
I. calculate the similarity of the finger printing and the standard finger-print of Xingdan injection to be measured, should be 0.80～1.00;
II. in the Xingdan injection finger printing to be measured, non-total peak area must not surpass 10% of total peak area;
The odds ratio that each total peak area in the ratio of 20%～80% total peak area and the standard finger-print arranged in the Xingdan injection finger printing III. to be measured, its difference must not be greater than ± 50%.
Be preferably:
A, the test of employing liquid chromatography are characterized as main finger printing with Radix Salviae Miltiorrhizae and Folium Ginkgo flavone constituents:
(1) preparation of need testing solution: it is an amount of that precision takes by weighing the red ejection preparation of Fructus Pruni to be measured, adds water and make the solution that every 1ml contains 10mg, with the microporous filter membrane filtration of 0.45 μ m, gets subsequent filtrate as need testing solution;
(2) preparation of object of reference solution: it is an amount of that precision takes by weighing the danshensu sodium reference substance, adds methanol and make the solution that every 1ml contains 15 μ g, as object of reference solution;
(3) chromatographic condition: the chromatographic column adopting octadecylsilane chemically bonded silica is a filler; Mobile phase A is 0.026% phosphoric acid solution, and Mobile phase B is an acetonitrile, gradient elution, and solvent ratios is from 0 minute to 30 minutes, and the ratio of Mobile phase B rises to 22% by 2%, and from 30 minutes to 60 minutes, the ratio of Mobile phase B rose to 26% by 22%; Flow velocity is 1.0ml/min, and the detection wavelength is 280 ± 2nm, and column temperature is 30 ℃;
(4) formulation of standard finger-print: the means of testing that is characterized as main finger printing with said method as formulation with Radix Salviae Miltiorrhizae and Folium Ginkgo flavone constituents; According to 10 batches or 10 batches of collection of illustrative plates that above test sample is measured, formulating standard finger-print, is benchmark with the retention time of the object of reference chromatographic peak determined, calculates the relative retention time of other total chromatographic peak, in the described standard finger-print, total peak has 3～30;
(5) with the described method in (1)～(3) as the means of testing that is characterized as main finger printing in the Xingdan injection to be measured with Radix Salviae Miltiorrhizae and Folium Ginkgo flavone constituents, the preparation testing sample finger printing;
(6) with the contrast of Xingdan injection finger printing to be measured and above-mentioned standard finger-print, in should meeting the following requirements partly or entirely:
I. calculate the similarity of the finger printing and the standard finger-print of Xingdan injection to be measured, should be 0.90～1.00;
II. in the Xingdan injection finger printing to be measured, non-total peak area must not surpass 5% of total peak area;
The odds ratio that each total peak area in the ratio of 10%～40% total peak area and the standard finger-print arranged in the Xingdan injection finger printing III. to be measured, its difference must not be greater than ± 30%;
B, employing liquid chromatography are tested the finger printing based on Folium Ginkgo terpene lactone composition characteristics:
(1) preparation of need testing solution: get the red ejection preparation 1.5g of Fructus Pruni to be measured, add water 40ml dissolving, add 5 of 2% hydrochloric acid solutions, with ethyl acetate extraction 4 times, merge extractive liquid, with 5% sodium acetate solution 20ml washing, divides and gets sodium acetate liquid, wash with ethyl acetate 10ml, merge ethyl acetate extraction liquid and washing liquid, wash with water 2 times, each 20ml, merge water lotion, with ethyl acetate 10ml washing, merge ethyl acetate liquid, reclaim ethyl acetate to doing, residue adds acetone makes dissolving also quantitatively be transferred in the 5ml measuring bottle in right amount, add acetone to scale, shake up, filter, filter, get subsequent filtrate as need testing solution;
(2) preparation of object of reference solution: get the ginkalide A reference substance, add methanol and make the solution that every 1ml contains 1mg, as object of reference solution;
(3) chromatographic condition: the chromatographic column adopting octadecylsilane chemically bonded silica is a filler: mobile phase A is methanol-oxolane (25: 10), Mobile phase B is a water, gradient elution, solvent ratios is from 0 minute to 25 minutes, the ratio of Mobile phase B is 65%, and from 25 minutes to 60 minutes, the ratio of Mobile phase B reduced to 35% by 65%, flow velocity is that 0.8ml/min, evaporative light scattering detector detect 30 ℃ of column temperatures;
(4) formulation of standard finger-print: the means of testing that is characterized as main finger printing with said method as formulation with Folium Ginkgo terpene lactone constituents; According to 10 batches or 10 batches of collection of illustrative plates that above test sample is measured, formulating standard finger-print, is benchmark with the retention time of the object of reference chromatographic peak determined, calculates the relative retention time of other total chromatographic peak, in the described standard finger-print, total peak has 3～20;
(5) with the described method in (1)～(3) as the means of testing that is characterized as main finger printing in the Xingdan injection to be measured with Folium Ginkgo terpene lactone constituents, the preparation testing sample finger printing;
(6) with the finger printing of Xingdan injection to be measured and the contrast of above-mentioned standard finger-print, in should meeting the following requirements partly or entirely:
I. calculate the similarity of the finger printing and the standard finger-print of Xingdan injection to be measured, should be 0.90～1.00;
II. in the Xingdan injection finger printing to be measured, non-total peak area must not surpass 5% of total peak area;
The odds ratio that each total peak area in the ratio of 30%～60% total peak area and the standard finger-print arranged in the Xingdan injection finger printing III. to be measured, its difference must not be greater than ± 30%.
Compared with prior art, the present invention's Xingdan injection product quality made from medical material or its extract of Folium Ginkgo and Radix Salviae Miltiorrhizae of perfect control more.This product composition complexity, if only with wherein one, two kind of composition illustrate its inherent quality, has certain one-sidedness, more can't judge the index components of its drug effect, be preferably on the stronger qualitative and quantitative analysis basis of specificity to increase and be characterized as main finger printing and control the quality of injection based on the finger printing of Radix Salviae Miltiorrhizae composition characteristics comprehensively with ginkgo leaf component; Because two kinds of medical material ingredients interference effect each other in the Xingdan injection, cause the finger printing characteristic peak of the more independent gingko leaf preparation of said preparation, red sage formulation to be very different, adopt the conventional detection Folium Ginkgo or the liquid phase chromatogram condition of Radix Salviae Miltiorrhizae, the separating effect at each composition characteristics peak is difficult to meet the demands, has only the condition of the present invention of employing, select for use suitable parameter to carry out gradient elution, just can obtain exclusive, accurate, stable, workable ideal finger printing.Proof by experiment, method of quality control of the present invention is more effective to the quality control of the Chinese medicine injection products made with Folium Ginkgo, Radix Salviae Miltiorrhizae, and method precision, stability are all higher.
Experimental example 1 is characterized as the preparation of main finger printing with Radix Salviae Miltiorrhizae and Folium Ginkgo flavone constituents
A, experimental apparatus, reagent and sample:
Reference substance: danshensu sodium: Nat'l Pharmaceutical ﹠ Biological Products Control Institute
B, chromatographic condition and system suitability experiment:
1. the selection of chromatographic column:
In the research process, having selected conventional octadecylsilane chemically bonded silica for use is the liquid-phase chromatographic column of filler, tried out Zorbax, Inertsil ODS-3 respectively, Diamonsil ODS (is C18,4.6mm * 200mm, 5 μ m) chromatographic column of three kinds of trades mark, the result shows that the chromatographic column of three kinds of trades mark all can reach separating effect preferably, and wherein Inertsil ODS-3 chromatographic column separating effect is best, and post is imitated the highest.So finally selecting Diamonsil ODS chromatographic column (4.6mm * 200mm, 5 μ m) for use is the experimentation post.
2. the selection of mobile phase:
Investigated (1) methanol in the research process respectively--water (10: 90), (2) methanol--0.1% glacial acetic acid (5: 95), (3) methanol--four kinds of flow phase system of 0.05% phosphoric acid (5: 995) (4) acetonitrile-0.026% phosphate aqueous solution (gradient elution).The result shows that peak shape is relatively poor under mobile phase (1) condition, separates bad; Under mobile phase (2) condition, peak shape is better, but it is less to go out the peak in 1 hour, goes out the peak after still having many components to be trapped in; Under mobile phase (3) condition, peak shape is better, and it is incomplete to go out the peak; Under mobile phase (4) condition, peak shape is better, goes out the peak fully and be evenly distributed, so finally selected.
3. detection wavelength determination:
In the research under acetonitrile-0.026% phosphoric acid (gradient elution) mobile phase condition, investigated the chromatographic peak situation under different-waveband typical wavelengths 205,230,254,280,360nm respectively, the result shows, chromatographic peak is less 205,230, under the 360nm, 205, baseline drift is serious under the 230nm, 254, baseline is good under the 288nm, and wherein chromatographic peak is more under the 288nm, so finally select for use 280nm as detecting wavelength.
4. instrument, chromatographic column and integral parameter:
4.1 instrument parameter: selected liquid-phase chromatographic analysis field mainstream configuration and well behaved Agilent 1100 series of high efficiency chromatograph of liquid for use, the Chemstation chromatographic work station.Chromatographic column is Diamonsil ODS (200mm * 4.6mm, 5 μ m); 30 ℃ of column temperatures, flow velocity 1.0ml/min.
4.2 integral parameter: Slope Sensitivity:1, peak width:0.05, smallest peaks area are 5% of object of reference (S) peak-to-peak area, minimum peak height be the S peak-to-peak high 5%.So setting can be avoided some very calculating of the chromatographic peak of small size (unimodal area accounts for total peak area less than 0.5%), guarantees the dependency with object of reference simultaneously.
5. the preparation of need testing solution:
Get the about 0.1g of this product, the accurate title, decide, and puts in the 10ml measuring bottle, and thin up shakes up to scale.With the filtering with microporous membrane of 0.45 Jing, get subsequent filtrate promptly.
6. the preparation of object of reference solution:
Danshensu sodium is one of main water-soluble active ingredient of Radix Salviae Miltiorrhizae, its integral area proportion in finger printing more greatly and more stable is relatively taken into account the research of intermediate and crude drug simultaneously, and therefore selected danshensu sodium is as object of reference, and using water as solvent, measurement result shows that this method is feasible.
7. finger printing and technical parameter:
Formulate standard finger-print according to 10 batch samples, test sample finger printing and standard finger-print are compared, similarity is all between 0.90～1.00.
Experimental example 2 is based on the preparation of the finger printing of Folium Ginkgo terpene lactone composition characteristics
A, experimental apparatus, reagent and sample:
Reference substance: ginkalide A: Nat'l Pharmaceutical ﹠ Biological Products Control Institute.
B, chromatographic condition and system suitability experiment:
1. the selection of chromatographic column:
In the research process, having selected conventional octadecylsilane chemically bonded silica for use is the liquid-phase chromatographic column of filler, tried out Zorbax (C18 respectively, 4.6mm * 200mm, 5um), Inertsil ODS-3 (C18,4.6mm * 200mm, 5um), PlatinumC18 (the chromatographic column of 4.6 * 250mm) three kinds of trades mark of 5 μ m, the result shows that the chromatographic column of three kinds of trades mark all can reach separating effect preferably, wherein (5 μ m, 4.6 * 250mm) chromatographic column separating effects are best for Platinum C18, post is imitated the highest, can reach more than 5000 (to calculate with the object of reference ginkalide A).So (5 μ m 4.6 * 250mm) are the experimentation post finally to select Platinum C18 for use.
2. the selection of mobile phase:
Investigated (1) methanol in the research process respectively--water (20: 80), (2) acetonitrile--water (20: 80), (3) acetonitrile--1% glacial acetic acid aqueous solution (gradient elution) (4) A is methanol-oxolane (25: 10), and B is four kinds of flow phase system of water (gradient elution).The result shows that peak shape is relatively poor under mobile phase (1) condition, and it is less to go out the peak in 1 hour, goes out the peak after still having many components to be trapped in; Under mobile phase (2) the mobile phase condition, peak shape is relatively poor, separates bad; (3) under the condition, the peak hangover is serious, and it is incomplete to go out the peak; Under mobile phase (4) condition, peak shape is better, goes out the peak fully and be evenly distributed, so finally selected.
3. detection wavelength determination:
Be methanol-oxolane (25: 10) at A in the research, B is under water (gradient elution) the mobile phase condition, the chromatographic peak under drift tube temperature (105 ℃, 110 ℃, 115 ℃) and air velocity (2.4ml/min, 2.7ml/min, the 3.0ml/min) condition and the situation of baseline noise have been investigated respectively, the result shows, steady at 110 ℃ of drift tube temperatures, air velocity 2.7ml/min baseline, noise is less, chromatographic peak separation and retention time are moderate and stable, so finally select for use 110 ℃ of drift tube temperatures, air velocity 2.7ml/min as testing conditions.
4. instrument, chromatographic column and integral parameter:
4.1 instrument parameter: selected liquid-phase chromatographic analysis field mainstream configuration and well behaved Alltech high performance liquid chromatograph for use, AlltechStation chromatographic work station, Alltech ELSD 2000ES.Chromatographic column is Platinum C18 (5 μ m 4.6 * 250mm); 30 ℃ of column temperatures, flow velocity 0.8ml/min.
4.2 integral parameter: Slope Sensitivity:500, peak width:0.2, smallest peaks area are 5% of object of reference (S) peak-to-peak area, minimum peak height be the S peak-to-peak high 5%.So setting can be avoided some very calculating of the chromatographic peak of small size (unimodal area accounts for total peak area less than 0.5%), guarantees the dependency with object of reference simultaneously.
5. the preparation of need testing solution:
Precision takes by weighing the about 1.5g of this product powder, adds water 40ml dissolving, adds 5 of 2% hydrochloric acid solutions, extract 4 times (15ml, 10ml, 10ml, 10ml) with the ethyl acetate jolting, merge extractive liquid, washs with 5% sodium acetate solution 20ml, divide and get sodium acetate liquid, with ethyl acetate 10ml washing.Merge ethyl acetate extraction liquid and washing liquid, wash with water 2 times, each 20ml merges water lotion, with ethyl acetate 10ml washing, merge ethyl acetate liquid, reclaim ethyl acetate to doing, residue adds acetone to be made dissolving and is transferred in the 5ml measuring bottle, add acetone to scale, shake up, promptly.
6. the preparation of object of reference solution:
Ginkalide A is one of main active in the Radix Salviae Miltiorrhizae, and its integral area proportion in finger printing more greatly and more stable is taken into account the research of intermediate and medical material simultaneously, and therefore selected ginkalide A is as object of reference.
7. finger printing and technical parameter:
Formulate standard finger-print according to 10 batch samples, test sample finger printing and standard finger-print are compared, similarity is all between 0.90～1.00.
The specific embodiment
Embodiment 1: adopt in the red freeze-dried powder of liquid chromatography for measuring Fructus Pruni and be characterized as main finger printing with Radix Salviae Miltiorrhizae and Folium Ginkgo flavone constituents:
(1) preparation of need testing solution: it is an amount of that precision takes by weighing the red freeze-dried powder of Fructus Pruni to be measured, adds water and make the solution that every 1ml contains 10mg, with the microporous filter membrane filtration of 0.45 μ m, gets subsequent filtrate as need testing solution;
(2) preparation of object of reference solution: it is an amount of that precision takes by weighing the danshensu sodium reference substance, adds methanol and make the solution that every 1ml contains 15 μ g, as object of reference solution;
(3) chromatographic condition: the chromatographic column adopting octadecylsilane chemically bonded silica is a filler; Mobile phase A is 0.026% phosphoric acid solution, and Mobile phase B is an acetonitrile, gradient elution, and solvent ratios is from 0 minute to 30 minutes, and the ratio of Mobile phase B rises to 22% by 2%, and from 30 minutes to 60 minutes, the ratio of Mobile phase B rose to 26% by 22%; Flow velocity is 1.0ml/min, and the detection wavelength is 280 ± 2nm, and column temperature is 30 ℃;
(4) formulation of standard finger-print: the means of testing that is characterized as main finger printing with said method as formulation with Radix Salviae Miltiorrhizae and Folium Ginkgo flavone constituents; According to 10 batches or 10 batches of collection of illustrative plates that above test sample is measured, formulate standard finger-print, be benchmark with the retention time of the object of reference chromatographic peak determined, calculate the relative retention time of other total chromatographic peak, in the described standard finger-print, total peak has 23;
(5) with the described method in (1)～(3) as the means of testing that is characterized as main finger printing in the Xingdan injection to be measured with Radix Salviae Miltiorrhizae and Folium Ginkgo flavone constituents, the preparation testing sample finger printing;
(6) with Xingdan injection finger printing to be measured and the contrast of above-mentioned standard finger-print, meet the following requirements:
Calculating the similarity of the finger printing and the standard finger-print of Xingdan injection to be measured, is 0.90～1.00.
Embodiment 2: adopt in the red freeze-dried powder of liquid chromatography for measuring Fructus Pruni the finger printing based on Folium Ginkgo terpene lactone composition characteristics:
(1) preparation of need testing solution: get the red freeze-dried powder 1.5g of Fructus Pruni to be measured, add water 40ml dissolving, add 5 of 2% hydrochloric acid solutions, with ethyl acetate extraction 4 times, merge extractive liquid, with 5% sodium acetate solution 20ml washing, divides and gets sodium acetate liquid, wash with ethyl acetate 10ml, merge ethyl acetate extraction liquid and washing liquid, wash with water 2 times, each 20ml, merge water lotion, with ethyl acetate 10ml washing, merge ethyl acetate liquid, reclaim ethyl acetate to doing, residue adds acetone makes dissolving also quantitatively be transferred in the 5ml measuring bottle in right amount, add acetone to scale, shake up, filter, filter, get subsequent filtrate as need testing solution;
(2) preparation of object of reference solution: get the ginkalide A reference substance, add methanol and make the solution that every 1ml contains 1mg, as object of reference solution;
(3) chromatographic condition: the chromatographic column adopting octadecylsilane chemically bonded silica is a filler: mobile phase A is methanol-oxolane (25: 10), Mobile phase B is a water, gradient elution, solvent ratios is from 0 minute to 25 minutes, the ratio of Mobile phase B is 65%, and from 25 minutes to 60 minutes, the ratio of Mobile phase B reduced to 35% by 65%, flow velocity is that 0.8ml/min, evaporative light scattering detector detect 30 ℃ of column temperatures;
(4) formulation of standard finger-print: the means of testing that is characterized as main finger printing with said method as formulation with Folium Ginkgo terpene lactone constituents; According to 10 batches or 10 batches of collection of illustrative plates that above test sample is measured, formulate standard finger-print, be benchmark with the retention time of the object of reference chromatographic peak determined, calculate the relative retention time of other total chromatographic peak, in the described standard finger-print, total peak has 9;
(5) with the described method in (1)～(3) as the means of testing that is characterized as main finger printing in the Xingdan injection to be measured with Folium Ginkgo terpene lactone constituents, the preparation testing sample finger printing;
(6) with the finger printing and the contrast of above-mentioned standard finger-print of Xingdan injection to be measured, meet the following requirements:
Calculating the similarity of the finger printing and the standard finger-print of Xingdan injection to be measured, is 0.90～1.00.
Embodiment 3: adopt in the red injection of liquid chromatography for measuring Fructus Pruni and be characterized as main finger printing with Radix Salviae Miltiorrhizae and Folium Ginkgo flavone constituents:
(1) preparation of need testing solution: it is an amount of that precision takes by weighing the red injection of Fructus Pruni to be measured, adds water and make the solution that every 1ml contains 10mg, with the microporous filter membrane filtration of 0.45 μ m, gets subsequent filtrate as need testing solution;
(2) preparation of object of reference solution: it is an amount of that precision takes by weighing protocatechualdehyde, adds water and make the solution that every 1ml contains 15 μ g, as object of reference solution;
(3) chromatographic condition: the chromatographic column adopting octadecylsilane chemically bonded silica is a filler; Mobile phase A is 1% glacial acetic acid solution, and Mobile phase B is an acetonitrile, gradient elution, and solvent ratios is from 0 minute to 30 minutes, and the ratio of Mobile phase B rises to 20% by 3%, and from 30 minutes to 75 minutes, the ratio of Mobile phase B rose to 26% by 20%; Flow velocity is 1.0ml/min, and the detection wavelength is 280 ± 2nm, and column temperature is 30 ℃;
(4) formulation of standard finger-print: the means of testing that is characterized as main finger printing with said method as formulation with Radix Salviae Miltiorrhizae and Folium Ginkgo flavone constituents; According to 10 batches or 10 batches of collection of illustrative plates that above test sample is measured, formulate standard finger-print, be benchmark with the retention time of the object of reference chromatographic peak determined, calculate the relative retention time of other total chromatographic peak, in the described standard finger-print, total peak has 21;
(5) with the described method in (1)～(3) as the means of testing that is characterized as main finger printing in the Xingdan injection to be measured with Radix Salviae Miltiorrhizae and Folium Ginkgo flavone constituents, the preparation testing sample finger printing;
(6) with Xingdan injection finger printing to be measured and the contrast of above-mentioned standard finger-print, meet the following requirements:
I. calculating the similarity of the finger printing and the standard finger-print of Xingdan injection to be measured, is 0.90～1.00;
II. in the Xingdan injection finger printing to be measured, non-total peak area is no more than 5% of total peak area;
The odds ratio that each total peak area in the ratio of 10%～40% total peak area and the standard finger-print arranged in the Xingdan injection finger printing III. to be measured, its difference is not more than ± 30%.
Embodiment 4: adopt in the red injection of liquid chromatography for measuring Fructus Pruni the finger printing based on Folium Ginkgo terpene lactone composition characteristics:
(1) preparation of need testing solution: get the red injection 1.5g of Fructus Pruni to be measured, add water 40ml dissolving, add 5 of 5% hydrochloric acid solutions, with n-butanol extraction 4 times, merge extractive liquid, with 2% sodium acetate solution 20ml washing, divides and gets sodium acetate liquid, wash with n-butyl alcohol 10ml, merge n-butanol extracting liquid and washing liquid, wash with water 2 times, each 20ml, merge water lotion, with n-butyl alcohol 10ml washing, merge n-butyl alcohol liquid, reclaim n-butyl alcohol to doing, residue adds methanol makes dissolving also quantitatively be transferred in the 5ml measuring bottle in right amount, add acetone to scale, shake up, filter, filter, get subsequent filtrate as need testing solution;
(2) preparation of object of reference solution: get the bilobalide reference substance, add methanol and make the solution that every 1ml contains 1mg, as object of reference solution;
(3) chromatographic condition: the chromatographic column adopting octadecylsilane chemically bonded silica is a filler: mobile phase A is acetonitrile-oxolane (22: 13), Mobile phase B is a water, gradient elution, solvent ratios is from 0 minute to 30 minutes, the ratio of Mobile phase B is 68%, and from 30 minutes to 60 minutes, the ratio of Mobile phase B reduced to 35% by 68%, flow velocity is that 0.9ml/min, evaporative light scattering detector detect 30 ℃ of column temperatures;
(4) formulation of standard finger-print: the means of testing that is characterized as main finger printing with said method as formulation with Folium Ginkgo terpene lactone constituents; According to 10 batches or 10 batches of collection of illustrative plates that above test sample is measured, formulate standard finger-print, be benchmark with the retention time of the object of reference chromatographic peak determined, calculate the relative retention time of other total chromatographic peak, in the described standard finger-print, total peak has 11;
(5) with the described method in (1)～(3) as the means of testing that is characterized as main finger printing in the Xingdan injection to be measured with Folium Ginkgo terpene lactone constituents, the preparation testing sample finger printing;
(6) with the finger printing and the contrast of above-mentioned standard finger-print of Xingdan injection to be measured, meet the following requirements:
I. calculating the similarity of the finger printing and the standard finger-print of Xingdan injection to be measured, is 0.90～1.00;
II. in the Xingdan injection finger printing to be measured, non-total peak area is no more than 5% of total peak area;
The odds ratio that each total peak area in the ratio of 30%～60% total peak area and the standard finger-print arranged in the Xingdan injection finger printing III. to be measured, its difference is not more than ± 30%.
Embodiment 5: adopt in the red glucose infusion liquid agent of liquid chromatography for measuring Fructus Pruni and be characterized as main finger printing with Radix Salviae Miltiorrhizae and Folium Ginkgo flavone constituents:
(1) preparation of need testing solution: precision is measured the red infusion solution 10ml of Fructus Pruni, with the microporous filter membrane filtration of 0.45 μ m, gets subsequent filtrate as need testing solution;
(2) preparation of object of reference solution: it is an amount of that precision takes by weighing salvianolic acid B, adds 75% methanol and make the solution that every 1ml contains 0.1mg, as object of reference solution;
(3) chromatographic condition: the chromatographic column adopting octadecylsilane chemically bonded silica is a filler; Mobile phase A is 0.05% phosphoric acid solution, and Mobile phase B is a methanol, gradient elution, and solvent ratios is from 0 minute to 25 minutes, and the ratio of Mobile phase B rises to 30% by 5%, and from 25 minutes to 60 minutes, the ratio of Mobile phase B rose to 35% by 25%; Flow velocity is 1.0ml/min, and the detection wavelength is 280 ± 2nm, and column temperature is 30 ℃;
(4) formulation of standard finger-print: the means of testing that is characterized as main finger printing with said method as formulation with Radix Salviae Miltiorrhizae and Folium Ginkgo flavone constituents; According to 10 batches or 10 batches of collection of illustrative plates that above test sample is measured, formulate standard finger-print, be benchmark with the retention time of the object of reference chromatographic peak determined, calculate the relative retention time of other total chromatographic peak, in the described standard finger-print, total peak has 20;
(5) with the described method in (1)～(3) as the means of testing that is characterized as main finger printing in the red infusion solution of Fructus Pruni to be measured with Radix Salviae Miltiorrhizae and Folium Ginkgo flavone constituents, the finger printing of preparation testing sample;
(6) with red infusion solution finger printing of Fructus Pruni to be measured and the contrast of above-mentioned standard finger-print, meet the following requirements:
I. calculating the finger printing of the red infusion solution of Fructus Pruni to be measured and the similarity of standard finger-print, is 0.90～1.00;
II. in the red infusion solution finger printing of Fructus Pruni to be measured, non-total peak area is no more than 5% of total peak area.
Embodiment 6: adopt in the red injection of liquid chromatography for measuring Fructus Pruni the finger printing based on Folium Ginkgo terpene lactone composition characteristics:
(1) preparation of need testing solution: precision is measured the red injection 30ml of Fructus Pruni, add 5 of 5% hydrochloric acid solutions, use chloroform extraction 4 times, merge extractive liquid,, wash with 5% sodium acetate solution 20ml, divide and get sodium acetate liquid, propose the 10ml washing, merge chloroform and put forward extracting solution and washing liquid with chloroform, wash with water 2 times, each 20ml merges water lotion, proposes the 10ml washing with chloroform, merge the chloroform extract, reclaim chloroform and carry to doing, residue adds ethanol makes dissolving also quantitatively be transferred in the 5ml measuring bottle in right amount, adds ethanol to scale, shake up, filter, filter, get subsequent filtrate as need testing solution;
(2) preparation of object of reference solution: get the ginkalide B reference substance, add ethanol and make the solution that every 1ml contains 1mg, as object of reference solution;
(3) chromatographic condition: the chromatographic column adopting octadecylsilane chemically bonded silica is a filler: mobile phase A is methanol-oxolane (25: 10), Mobile phase B is a water, gradient elution, solvent ratios is from 0 minute to 25 minutes, the ratio of Mobile phase B is 65%, and from 25 minutes to 60 minutes, the ratio of Mobile phase B reduced to 35% by 65%, flow velocity is that 0.8ml/min, evaporative light scattering detector detect 30 ℃ of column temperatures;
(4) formulation of standard finger-print: the means of testing that is characterized as main finger printing with said method as formulation with Folium Ginkgo terpene lactone constituents; According to 10 batches or 10 batches of collection of illustrative plates that above test sample is measured, formulate standard finger-print, be benchmark with the retention time of the object of reference chromatographic peak determined, calculate the relative retention time of other total chromatographic peak, in the described standard finger-print, total peak has 7;
(5) with the described method in (1)～(3) as the means of testing that is characterized as main finger printing in the red injection of Fructus Pruni to be measured with Folium Ginkgo terpene lactone constituents, the finger printing of preparation testing sample;
(6) with the finger printing and the contrast of above-mentioned standard finger-print of the red injection of Fructus Pruni to be measured, meet the following requirements:
I. calculating the finger printing of the red injection of Fructus Pruni to be measured and the similarity of standard finger-print, is 0.90～1.00;
II. in the red injection finger printing of Fructus Pruni to be measured, non-total peak area is no more than 5% of total peak area.
Claims (4)
1. the detection method of an Xingdan injection, described preparation is by the Folium Ginkgo medical material: red rooted salvia=20-80:80-20 prescription, difference or merging adopt water or alcoholic solution to extract, carry out suitably refining, mixing with in the sedimentation method, column chromatography, solvent extraction and the supercritical extraction one or more then, make injection then; Perhaps by Folium Ginkgo extract: the injection that Radix Salviae Miltiorrhizae extract=the 20-80:80-20 prescription is made; Described extract derives from commercially available or adopts water extraction or adopt alcoholic solution to extract, and carries out suitably refining obtaining afterwards with in the sedimentation method, column chromatography, solvent extraction and the supercritical extraction one or more then; It is characterized in that: this method comprises following content:
The test of the finger printing of Xingdan injection comprises with Radix Salviae Miltiorrhizae and Folium Ginkgo flavone constituents being characterized as main finger printing and based in the finger printing of Folium Ginkgo terpene lactone composition characteristics one or both.
2. according to the detection method of the described Xingdan injection of claim 1, it is characterized in that this method comprises one or both in the following finger printing:
A, the test of employing liquid chromatography are characterized as main finger printing with Radix Salviae Miltiorrhizae and Folium Ginkgo flavone constituents:
(1) preparation of need testing solution: it is an amount of to get the red ejection preparation of Fructus Pruni to be measured, adds water or methanol or dissolve with ethanol or dilution, shakes up, and filters, and gets subsequent filtrate as need testing solution;
(2) preparation of object of reference solution: get the main active reference substance in an amount of Radix Salviae Miltiorrhizae and the Folium Ginkgo medical material, comprise a kind of in danshensu sodium, protocatechualdehyde, salvianolic acid B or its magnesium salt, Quercetin, kaempferide, the isorhamnetin, water or methanol or dissolve with ethanol, be settled to suitable concn, as object of reference solution;
(3) chromatographic condition: the chromatographic column adopting octadecylsilane chemically bonded silica is a filler: mobile phase is acetonitrile or methanol-0.01mol/L～2mol/L biphosphate sodium water solution or 0.01mol/L～2mol/L potassium dihydrogen phosphate aqueous solution or 0.01mol/L～2mol/L sodium hydrogen phosphate aqueous solution or water or 0.1%～5% glacial acetic acid solution or 0.1%～5% formic acid solution or 0.02%～5% phosphoric acid solution, gradient elution, flow velocity is 0.5～2.0ml/min, one or several or the evaporation photodetector that detect wavelength and be in 190～410nm scope detect, and column temperature is in 20～60 ℃ of scopes;
(4) formulation of standard finger-print: the means of testing that is characterized as main finger printing with said method as formulation with Radix Salviae Miltiorrhizae and Folium Ginkgo flavone constituents; According to 10 batches or 10 batches of collection of illustrative plates that above test sample is measured, formulating standard finger-print, is benchmark with the retention time of the object of reference chromatographic peak determined, calculates the relative retention time of other total chromatographic peak, in the described standard finger-print, total peak has 3～50;
(5) with the described method in (1)～(3) as the means of testing that is characterized as main finger printing in the Xingdan injection to be measured with Radix Salviae Miltiorrhizae and Folium Ginkgo flavone constituents, the preparation testing sample finger printing;
(6) with the finger printing and the contrast of above-mentioned standard finger-print of Xingdan injection to be measured, should meet the following requirements:
I. calculate the similarity of the finger printing and the standard finger-print of Xingdan injection to be measured, should be 0.80～1.00;
II. in the Xingdan injection finger printing to be measured, non-total peak area must not surpass 10% of total peak area;
The odds ratio that each total peak area in the ratio of 5%～60% total peak area and the standard finger-print arranged in the Xingdan injection finger printing III. to be measured, its difference must not be greater than ± 50%;
B, employing liquid chromatography are tested the finger printing based on Folium Ginkgo terpene lactone composition characteristics:
(1) preparation of need testing solution: it is an amount of to get the red ejection preparation of Fructus Pruni to be measured, be dissolved in water, add 0.2%～30% hydrochloric acid solution, with ethyl acetate or n-butyl alcohol or chloroform or dichloromethane extraction, combining extraction liquid, wash with 0.5%～20% sodium acetate solution, divide and get sodium acetate liquid,, merge ethyl acetate or n-butyl alcohol or chloroform or dichloromethane extract and washing liquid with ethyl acetate or n-butyl alcohol or chloroform or washed with dichloromethane, wash with water, merge water lotion,, merge ethyl acetate or n-butyl alcohol or chloroform or dichloromethane solution with ethyl acetate or n-butyl alcohol or chloroform or washed with dichloromethane, reclaim ethyl acetate or n-butyl alcohol or chloroform or dichloromethane to doing, residue adds acetone or methanol or ethanol makes dissolving, shakes up, and filters, filter, get subsequent filtrate as need testing solution;
(2) preparation of object of reference solution: get a kind of in bilobalide or ginkalide A or ginkalide B or the ginkalide C, with methanol or dissolve with ethanol, be settled to suitable concn, as object of reference solution;
(3) chromatographic condition: the chromatographic column adopting octadecylsilane chemically bonded silica is a filler: mobile phase A is acetonitrile or acetonitrile-oxolane (5～95:95～5) or methanol or methanol-oxolane (5～95:95～5), Mobile phase B is water or 0.1%～5% glacial acetic acid or 0.1%～5% formic acid or 0.005%～5% phosphoric acid solution, gradient elution, flow velocity is 0.5～2.0ml/min, detect wavelength is that one or several or evaporative light scattering detector in 190～410nm scope detects, and column temperature is in 20～60 ℃ of scopes;
(4) formulation of standard finger-print: the means of testing that is characterized as main finger printing with said method as formulation with Folium Ginkgo terpene lactone constituents; According to 10 batches or 10 batches of collection of illustrative plates that above test sample is measured, formulating standard finger-print, is benchmark with the retention time of the object of reference chromatographic peak determined, calculates the relative retention time of other total chromatographic peak, in the described standard finger-print, total peak has 3～30;
(5) with the described method in (1)～(3) as the means of testing that is characterized as main finger printing in the Xingdan injection to be measured with Folium Ginkgo terpene lactone constituents, the preparation testing sample finger printing;
(6) with the finger printing of Xingdan injection to be measured and the contrast of above-mentioned standard finger-print, in should meeting the following requirements partly or entirely:
I. calculate the similarity of the finger printing and the standard finger-print of Xingdan injection to be measured, should be 0.80～1.00;
II. in the Xingdan injection finger printing to be measured, non-total peak area must not surpass 10% of total peak area;
The odds ratio that each total peak area in the ratio of 20%～80% total peak area and the standard finger-print arranged in the Xingdan injection finger printing III. to be measured, its difference must not be greater than ± 50%.
3. according to the detection method of the described Xingdan injection of claim 2, it is characterized in that this method comprises one or both in the following finger printing:
A, the test of employing liquid chromatography are characterized as main finger printing with Radix Salviae Miltiorrhizae and Folium Ginkgo flavone constituents:
(1) preparation of need testing solution: it is an amount of that precision takes by weighing the red ejection preparation of Fructus Pruni to be measured, adds water and make the solution that every 1ml contains 10mg, with the microporous filter membrane filtration of 0.45 μ m, gets subsequent filtrate as need testing solution;
(2) preparation of object of reference solution: it is an amount of that precision takes by weighing the danshensu sodium reference substance, adds methanol and make the solution that every 1ml contains 15 μ g, as object of reference solution;
(3) chromatographic condition: the chromatographic column adopting octadecylsilane chemically bonded silica is a filler; Mobile phase A is 0.026% phosphoric acid solution, and Mobile phase B is an acetonitrile, gradient elution, and solvent ratios is from 0 minute to 30 minutes, and the ratio of Mobile phase B rises to 22% by 2%, and from 30 minutes to 60 minutes, the ratio of Mobile phase B rose to 26% by 22%; Flow velocity is 1.0ml/min, and the detection wavelength is 280 ± 2nm, and column temperature is 30 ℃;
(4) formulation of standard finger-print: the means of testing that is characterized as main finger printing with said method as formulation with Radix Salviae Miltiorrhizae and Folium Ginkgo flavone constituents; According to 10 batches or 10 batches of collection of illustrative plates that above test sample is measured, formulating standard finger-print, is benchmark with the retention time of the object of reference chromatographic peak determined, calculates the relative retention time of other total chromatographic peak, in the described standard finger-print, total peak has 3～30;
(5) with the described method in (1)～(3) as the means of testing that is characterized as main finger printing in the Xingdan injection to be measured with Radix Salviae Miltiorrhizae and Folium Ginkgo flavone constituents, the preparation testing sample finger printing;
(6) with Xingdan injection finger printing to be measured and the contrast of above-mentioned standard finger-print, should meet the following requirements:
I. calculate the similarity of the finger printing and the standard finger-print of Xingdan injection to be measured, should be 0.90～1.00;
II. in the Xingdan injection finger printing to be measured, non-total peak area must not surpass 5% of total peak area;
The odds ratio that each total peak area in the ratio of 10%～40% total peak area and the standard finger-print arranged in the Xingdan injection finger printing III. to be measured, its difference must not be greater than ± 30%;
B, employing liquid chromatography are tested the finger printing based on Folium Ginkgo terpene lactone composition characteristics:
(1) preparation of need testing solution: get the red ejection preparation 1.5g of Fructus Pruni to be measured, add water 40ml dissolving, add 5 of 2% hydrochloric acid solutions, with ethyl acetate extraction 4 times, merge extractive liquid, with 5% sodium acetate solution 20ml washing, divides and gets sodium acetate liquid, wash with ethyl acetate 10ml, merge ethyl acetate extraction liquid and washing liquid, wash with water 2 times, each 20ml, merge water lotion, with ethyl acetate 10ml washing, merge ethyl acetate liquid, reclaim ethyl acetate to doing, residue adds acetone makes dissolving also quantitatively be transferred in the 5ml measuring bottle in right amount, add acetone to scale, shake up, filter, filter, get subsequent filtrate as need testing solution;
(2) preparation of object of reference solution: get the ginkalide A reference substance, add methanol and make the solution that every 1ml contains 1mg, as object of reference solution;
(3) chromatographic condition: the chromatographic column adopting octadecylsilane chemically bonded silica is a filler: mobile phase A is methanol-oxolane (25:10), Mobile phase B is a water, gradient elution, solvent ratios is from 0 minute to 25 minutes, the ratio of Mobile phase B is 65%, and from 25 minutes to 60 minutes, the ratio of Mobile phase B reduced to 35% by 65%, flow velocity is that 0.8ml/min, evaporative light scattering detector detect 30 ℃ of column temperatures;
(4) formulation of standard finger-print: the means of testing that is characterized as main finger printing with said method as formulation with Folium Ginkgo terpene lactone constituents; According to 10 batches or 10 batches of collection of illustrative plates that above test sample is measured, formulating standard finger-print, is benchmark with the retention time of the object of reference chromatographic peak determined, calculates the relative retention time of other total chromatographic peak, in the described standard finger-print, total peak has 3～20;
(5) with the described method in (1)～(3) as the means of testing that is characterized as main finger printing in the Xingdan injection to be measured with Folium Ginkgo terpene lactone constituents, the preparation testing sample finger printing;
(6) with the finger printing and the contrast of above-mentioned standard finger-print of Xingdan injection to be measured, should meet the following requirements:
I. calculate the similarity of the finger printing and the standard finger-print of Xingdan injection to be measured, should be 0.90～1.00;
II. in the Xingdan injection finger printing to be measured, non-total peak area must not surpass 5% of total peak area;
The odds ratio that each total peak area in the ratio of 30%～60% total peak area and the standard finger-print arranged in the Xingdan injection finger printing III. to be measured, its difference must not be greater than ± 30%.
4. according to the detection method of the described Xingdan injection of claim 1, it is characterized in that: described injection is the injection that is directly used in drug administration by injection, need to be used for after the dilution concentrated solution for injection of intravenous drip, directly for the glucose intravenous infusion of intravenous drip or sodium chloride intravenous infusion or the injectable sterile powder or the aseptic block that make with freeze-drying or spray drying method.
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