CN101637567A - Rhizoma ligustici wallichii quality control method in Chinese medicine preparation - Google Patents
Rhizoma ligustici wallichii quality control method in Chinese medicine preparation Download PDFInfo
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Abstract
The invention relates to a rhizoma ligustici wallichii quality control method in a Chinese medicine preparation, which belongs to the technical field of medicines. A Yixinshu Chinese medicine preparation comprises seven medicines of ginseng, rhizoma ligustici wallichii, salvia miltiorrhiza, radix ophiopogonis, shizandra, and the like, has the effects of tonifying Qi, recovering the pulse, promoting blood circulation, removing blood stasis, nourishing Yin and promoting the production of body fluid and can be widely used for clinically treating angina pectoris, myocardial ischemia, various kindsof arrhythmia cordis, atrial premature beats, thoracalgia, angina pectoris patients of a coronary heart disease, and the like at present. The rhizoma ligustici wallichii quality control method directly provides detection indexes, detection measures, technical methods, and the like for the quality of salvia miltiorrhiza in the relatively produced Yixinshu preparation in order to better control thequality of the Chinese medicine preparation, ensures safety and curative effect of medicine application, can better guide production and provide a high-quality product for consumers.
Description
Technical field:
The present invention relates to rhizoma ligustici wallichii quality control method in the YIXINSHU Chinese medicine preparation, belong to technical field of medicaments.
Background technology:
The YIXINSHU Chinese medicine preparation is to form with seven flavor medicines such as Radix Ginseng, Rhizoma Chuanxiong, Fructus Schisandrae Chinensis, Radix Salviae Miltiorrhizaes, has Yiqi and vein recovery, blood circulation promoting and blood stasis dispelling, the effect of YIN nourishing and the production of body fluid promoting, be used for deficiency of both QI and YIN, the cardiopalmus irregularly intermittent and regularly intermittent pulse does not uncomfortable in chestly relax, chest pain and angina pectoris are seen the person that has the above-mentioned symptom, are widely used in treatment angina pectoris, myocardial ischemia, various arrhythmia, artrial premature beat, chest pain and angina pectoris trouble etc. at present clinically.Pharmaceutical preparation must be on the basis that guarantees the constant product quality controllable safety, constantly more new development, so that better controlling the quality of this Chinese medicine preparation, thus must be controlled from the source, just can better guarantee the safety of medication.Nowadays, Chinese medicine preparation as the most potential drug resource by the whole world under the cognitive situation, the Chinese government has set up a series of policies widely and has dealt with the Chinese medicine compound preparation standardization, modern requirement.Wherein most important is exactly quality how to control Chinese medicine preparation.Our the most frequently used method is exactly to select main active or its index sexual element of Chinese crude drug at present, to the discriminating of these compositions and assay to reach the purpose of these Chinese medicine preparation quality of control.But this method of controlling at Chinese medicine and Chinese medicine preparation index composition can not science and comprehensively guaranteed the drug effect of Chinese medicine.Pharmacological action shows that Rhizoma Chuanxiong has has the abirritative effect to the central nervous system, has simultaneously to bring high blood pressure down, and peripheral vessels is had the effect of direct expansion.And the YIXINSHU Chinese medicine preparation is with the preparation of seven flavor medicine through being processed into such as Radix Ginseng, Rhizoma Chuanxiong, Fructus Schisandrae Chinensis, Radix Salviae Miltiorrhizaes, and is widely used in treatment angina pectoris, myocardial ischemia, various arrhythmia, artrial premature beat, chest pain and angina pectoris trouble etc. clinically.So the quality of Rhizoma Chuanxiong is directly connected to the curative effect of said preparation in the YIXINSHU preparation, thereby guarantee that for the raising of rhizoma ligustici wallichii quality control method the curative effect of YIXINSHU Chinese medicine preparation seems very necessary.
Summary of the invention
The objective of the invention is to: rhizoma ligustici wallichii quality control method in a kind of YIXINSHU Chinese medicine preparation is provided, and this method provides means, technical method of the index that detects, detection or the like to relevant production, testing agency; So that better control the quality of YIXINSHU Chinese medicine preparation, be the clinical YIXINSHU Chinese medicine preparation that a kind of determined curative effect is provided, guarantee the safety and the curative effect of medication, can better instruct production simultaneously, make the quality of consumer's energy full appreciation YIXINSHU Chinese medicine preparation.
The present invention relates to rhizoma ligustici wallichii quality control method in the YIXINSHU Chinese medicine preparation, it comprise Rhizoma Chuanxiong the place of production, collection, processing, differentiate, contain the index of survey project as Rhizoma Chuanxiong quality control in the said preparation.
Rhizoma ligustici wallichii quality control method in the above-mentioned YIXINSHU Chinese medicine preparation, adopt following partly or entirely:
(1) place of production of Rhizoma Chuanxiong is: ground such as Sichuan, Yunnan, Guizhou.
(2) acquisition time of Rhizoma Chuanxiong is: annual excavates in 4-10 month.
(3) the collection processing method of Rhizoma Chuanxiong is: the bright Rhizoma Chuanxiong that takes, remove earth, Ex-all stem and leaf and fibrous root, chip drying.
(4) discrimination method of the Radix Astragali is:
Method 1: adopt thin layer chromatography, generally use silica gel G or silica gel G F
254Or silica gel H is a lamellae, the point sample amount is arbitrary volume between 0.5～30 μ l, with the Rhizoma Chuanxiong control medicinal material, ligustrazine, ferulic acid, adenine, adenosine, all or part of kind product in contrast in the vanillin, sample pre-treatments comprises direct sample or with reconcentration method behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, developing solvent can be normal hexane, ethyl acetate, petroleum ether, Ethyl formate, formic acid, dimethylbenzene, toluene, one or more reagent of cyclohexane extraction are formulated according to a certain percentage, and the condition of inspecting comprises under the ultra-violet lamp inspects, put again under the ultra-violet lamp after ammonia is smoked and inspect, or spray is with the chromotropic acid sulfuric acid solution, the anisaldehyde sulfuric acid solution, iodine vapor, the method of 10% phosphomolybdic acid ethanol solution solution colour developing;
Method 2: adopt high performance liquid chromatography or evaporative light scattering detector and high performance liquid chromatography coupling method, sample pre-treatments comprises direct sample or with the method for reconcentration behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, use the chromatographic column of C8 or C18 type filler, with the second eyeball, water, one or more kind solvents in the methanol are mobile phase under the proper ratio condition of routine, with the Rhizoma Chuanxiong control medicinal material, ligustrazine, ferulic acid, adenine, adenosine, all or part of kind product in contrast in the vanillin detect wavelength in 200～600nm scope;
(6) Rhizoma Chuanxiong content adopts following method:
Method 1: adopt high performance liquid chromatography or employing evaporative light scattering detector and high performance liquid chromatography coupling method to measure ligustrazine in this product, ferulic acid, adenine, adenosine, all or part of kind in the vanillin, sample pre-treatments comprises direct sample or with reconcentration method behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, use the chromatographic column of C8 or C18 type filler, with methanol, water, the second eyeball, glacial acetic acid, oxolane, one or more kind solvents in the phosphoric acid solution are mobile phase under the proper ratio condition of routine, detect wavelength in 200～600nm scope;
Method 2: adopt TLC scanning method, generally use silica gel G or silica gel G F
254Or silica gel H is a lamellae, the point sample amount is arbitrary volume between 0.5～30 μ l, with the Rhizoma Chuanxiong control medicinal material, ligustrazine, ferulic acid, adenine, adenosine, all or part of kind product in contrast in the vanillin, sample pre-treatments comprises reconcentration method behind direct sample or ethanol or methanol or water or ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, developing solvent can be chloroform, methanol, ethyl acetate, petroleum ether, Ethyl formate, formic acid, dimethylbenzene, toluene, one or more reagent of cyclohexane extraction are formulated according to a certain percentage, put under the ultra-violet lamp or adopt ammonia smoked after put again and inspect under the ultra-violet lamp or spray method with chromotropic acid sulfuric acid solution or anisaldehyde sulfuric acid solution or iodine vapor or the colour developing of 10% phosphomolybdic acid ethanol solution, speckle adopts single wavelength or dual wavelength to scan on thin-layer chromatogram scanner, and scanning wavelength is 200～400nm;
Rhizoma ligustici wallichii quality control method in the above-mentioned YIXINSHU Chinese medicine preparation, adopt following method part or all of:
(1) place of production of Rhizoma Chuanxiong is: Sichuan, Yunnan, Guizhou province.
(2) acquisition time of Rhizoma Chuanxiong is: annual excavates in 6-9 month.
(3) the collection processing method of Rhizoma Chuanxiong is: the bright Rhizoma Chuanxiong that takes, remove earth, Ex-all stem and leaf and fibrous root, chip drying behind the moistening that is soaked in water.
(4) discrimination method of Rhizoma Chuanxiong is: adopt thin layer chromatography, use silica gel g thin-layer plate, the point sample amount is an a certain volume between 0.5 μ l～30 μ l, with the product in contrast of all or part of kind in Rhizoma Chuanxiong control medicinal material, the ferulic acid, sample pre-treatments is to use separately or the impurity of mixed solvent extraction according to a certain percentage with chloroform, ether, petroleum ether, use a kind of or dissolved method of they any mixed solvents in ethanol, methanol, ethyl acetate, the water then, developing solvent is normal hexane, ethyl acetate, and the condition of inspecting is that 365nm inspects under the ultra-violet lamp.
(5) Rhizoma Chuanxiong content adopts following method: adopt high performance liquid chromatography or employing evaporative light scattering detector and high performance liquid chromatography coupling method to measure ligustrazine in this product, all or part of kind in the ferulic acid, sample pre-treatments comprises direct sample or with reconcentration method behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, use the chromatographic column of C8 or C18 type filler, with methanol, water, the second eyeball, glacial acetic acid, oxolane, one or more kind solvents in the phosphoric acid solution are mobile phase under the proper ratio condition of routine, detect wavelength in 200～600nm scope;
Rhizoma ligustici wallichii quality control method in the above-mentioned YIXINSHU Chinese medicine preparation, adopt following method part or all of:
(1) place of production of Rhizoma Chuanxiong is: the area, Sichuan.
(2) the collection phase of Rhizoma Chuanxiong is: annual excavates in 8-9 month.
(3) the collection processing method of Rhizoma Chuanxiong is: the bright Rhizoma Chuanxiong that takes, remove earth, and Ex-all stem and leaf and fibrous root are soaked in water, and solarization is dried in the air, chip drying behind the moistening.
(4) discrimination method of Rhizoma Chuanxiong is: get this product content 20g, add ethyl acetate 60ml, reflux, extract, 30min filters, and filtrate is used 5%NaHNO
3Solution extraction 3 times merges the aqueous alkali layer, is acidified to pH1 with dilute sulfuric acid, with extracted with diethyl ether 3 times, combined ether layer, is recycled to driedly, adds methanol 1m and makes dissolving, as need testing solution.Other gets the Rhizoma Chuanxiong control medicinal material and prepares control medicinal material solution as stated above.Get the ferulic acid reference substance more in addition, add methanol and be mixed with the reference substance solution that contains 0.5mg among every 1ml.Draw each 10 μ l of above-mentioned solution respectively, point is on same silica gel G-CMC lamellae, with benzene-ethyl acetate-glacial acetic acid (4: 1: 0.3) is developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
(5) the survey method that contains of Rhizoma Chuanxiong is: the HPLC method is measured content of ferulic acid
Chromatographic condition chromatographic column KromasilC18; Mobile phase: second eyeball: 0.1% glacial acetic acid (18: 82) is a mobile phase; Flow velocity: 1mL/min; Detect wavelength: 320nm; Column temperature: 30 ℃; Theoretical cam curve is calculated by ferulic acid and is not less than 5000.
It is an amount of that the preparation precision of reference substance solution takes by weighing the ferulic acid reference substance, adds methanol one glacial acetic acid (99: 1) and be mixed with the solution that every 1mL contains 26.56ug respectively, shakes up, promptly.
The preparation precision of the need testing solution material powder 0.5g (cross No. 4 sieve) that gets it filled, put in the 50mL tool plug conical flask, accurate methanol one 2% sodium bicarbonate solution (95: the 5) 25mL that adds, ultrasonic 100min, put to room temperature, add methanol one 2% sodium bicarbonate solution (95: 5) and supply the weight that subtracts mistake, shake up, filter with microporous filter membrane (0.45um), promptly.
Accurate respectively above-mentioned reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly.
Compared with prior art, method of quality control provided by the invention can better, further be controlled a kind of product quality of YIXINSHU Chinese medicine preparation, guarantee the safety of medication, after using the present invention, the unit or the testing agency that produce this product are controlled from source raw material Rhizoma Chuanxiong, guarantee the curative effect of this YIXINSHU, can guarantee the quality of finished drug product; We find when testing: in order to reach the definite curative effect of YIXINSHU Chinese medicine preparation, just must begin from the source control, comprise Rhizoma Chuanxiong the place of production, collection, processing, differentiate, contain the survey project.So more help instruct producing, allow consumer's full appreciation product quality, this quasi drugs of relieved use.For the easy quality of controlling the Rhizoma Chuanxiong medical material all sidedly provides more efficiently analytical method.
Utilize Rhizoma Chuanxiong method of quality control provided by the invention for proof and can better control the product quality of YIXINSHU Chinese medicine preparation, the medicine that obtains has effective effect, and the applicant has carried out a series of experiments;
The investigation in the Rhizoma Chuanxiong place of production in the test example 1 YIXINSHU Chinese medicine preparation
This experiment is by measuring the quality of investigating different places of production Rhizoma Chuanxiong to the content of ferulic acid in the Szechwan Ligusticum wallichii of identical collection period and identical processing method, Yunnan Rhizoma Chuanxiong, the Guizhou Rhizoma Chuanxiong.
1.1 chromatographic condition chromatographic column KromasilC18; Mobile phase: second eyeball: 0.1% glacial acetic acid (18: 82) is a mobile phase; Flow velocity: 1mL/min; Detect wavelength: 320nm; Column temperature: 30 ℃; Theoretical cam curve is calculated by ferulic acid and is not less than 5000.
1.2 algoscopy
1.2.1 it is an amount of that the preparation precision of reference substance solution takes by weighing the ferulic acid reference substance, adds methanol one glacial acetic acid (99: 1) and be mixed with the solution that every 1mL contains 26.56ug respectively, shakes up, promptly.
The material powder 0.5g 1.2.2 the preparation precision of need testing solution is got it filled (crossing sieve No. 4), put in the 50mL tool plug conical flask, accurate methanol one 2% sodium bicarbonate solution (95: the 5) 25mL that adds, ultrasonic 100min, put to room temperature, add methanol one 2% sodium bicarbonate solution (95: 5) and supply the weight that subtracts mistake, shake up, filter with microporous filter membrane (0.45um), promptly.
1.2.3 measure accurate respectively above-mentioned reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly.
1.3 result and discussion
1.3.1 sample determination result
Different places of production Rhizoma Chuanxiong medical material sample, unit (%) the results are shown in Table 1 one 1
1.3.2 discuss
Result of study shows that the ferulic acid component content in the Rhizoma Chuanxiong of the different places of production differs greatly, and illustrates that interior variation of kind of different places of production medical material caused the difference of medical material quanlity.Wherein the Rhizoma Chuanxiong with Sichuan is good.
Rhizoma Chuanxiong is gathered the investigation in period in the test example 2 YIXINSHU Chinese medicine preparation
Experiment is investigated the Rhizoma Chuanxiong quality by the middle ferulaic acid content in the different acquisition phase Szechwan Ligusticum wallichii is measured.
2.1 chromatographic condition chromatographic column KromasilC18; Mobile phase: second eyeball: 0.1% glacial acetic acid (18: 82) is a mobile phase; Flow velocity: 1mL/min; Detect wavelength: 320nm; Column temperature: 30 ℃; Theoretical cam curve is calculated by ferulic acid and is not less than 5000.
2.2 algoscopy
2.2.1 it is an amount of that the preparation precision of reference substance solution takes by weighing the ferulic acid reference substance, adds methanol one glacial acetic acid (99: 1) and be mixed with the solution that every 1mL contains 26.56ug respectively, shakes up, promptly.
The material powder 0.5g 2.2.2 the preparation precision of need testing solution is got it filled (crossing sieve No. 4), put in the 50mL tool plug conical flask, accurate methanol one 2% sodium bicarbonate solution (95: the 5) 25mL that adds, ultrasonic 100min, put to room temperature, add methanol one 2% sodium bicarbonate solution (95: 5) and supply the weight that subtracts mistake, shake up, filter with microporous filter membrane (0.45um), promptly.
2.2.3 measure accurate respectively above-mentioned reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly.
2.3 result and discussion
2.3.1 result
Different acquisition phase Milkvetch Root sample, unit (%) the results are shown in Table 2 one 1
2.3.2 discuss
Result of study shows that the ferulic acid component content in the different acquisition phase Rhizoma Chuanxiong differs greatly, and illustrates that interior variation of kind of the medical material that the different acquisition phase gathers caused the difference of medical material quanlity.Its changes of contents is characterized as to be increased to gradually and reduces, so wherein the optimal acquisition phase is that the content that 8-9 gathers is up to good.
The study on the stability that Rhizoma Chuanxiong is differentiated in the test example 3 YIXINSHU Chinese medicine preparation
This experiment is learned investigation by 5 batches of Rhizoma Chuanxiongs being carried out discrimination method, to determine the stability of this method.
3.1 the preparation of standard solution
3.1.1 this product 10g is got in the preparation of need testing solution, adds ethyl acetate 60ml, reflux, extract, 30min filters, and filtrate is used 5%NaHNO
3Solution extraction 3 times merges the aqueous alkali layer, is acidified to pH1 with dilute sulfuric acid, with extracted with diethyl ether 3 times, combined ether layer, is recycled to driedly, adds methanol 1m and makes dissolving, as need testing solution.
3.1.2 getting the Rhizoma Chuanxiong control medicinal material, the preparation of reference substance solution solution prepares control medicinal material solution as stated above.Get the ferulic acid reference substance more in addition, add methanol and be mixed with the reference substance solution that contains 0.5mg among every 1ml.
3.1.3 differentiate and draw each 10 μ l of above-mentioned solution respectively, point is on same silica gel G-CMC lamellae, with benzene-ethyl acetate-glacial acetic acid (4: 1: 0.3) is developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
3.3 on test sample and control medicinal material and the corresponding position of reference substance chromatograph, show the speckle of same color as a result; Simultaneously 5 batch samples are all more stable, illustrate that the discrimination method that the method can be used as the Rhizoma Chuanxiong medical material carries out the discriminating of Rhizoma Chuanxiong medical material.
The Rhizoma Chuanxiong medical material contains the methodological study of survey in the test example 4 YIXINSHU Chinese medicine preparation
4.1 chromatographic condition chromatographic column KromasilC18; Mobile phase: second eyeball: 0.1% glacial acetic acid (18: 82) is a mobile phase; Flow velocity: 1mL/min; Detect wavelength: 320nm; Column temperature: 30 ℃; Theoretical cam curve is calculated by ferulic acid and is not less than 5000.
4.2 it is an amount of that the preparation precision of reference substance solution takes by weighing the ferulic acid reference substance, adds methanol one glacial acetic acid (99: 1) and be mixed with the solution that every 1mL contains 26.56ug respectively, shakes up, promptly.
The material powder 0.5g 4.3 the preparation precision of need testing solution is got it filled (crossing sieve No. 4), put in the 50mL tool plug conical flask, accurate methanol one 2% sodium bicarbonate solution (95: the 5) 25mL that adds, ultrasonic 100min, put to room temperature, add methanol one 2% sodium bicarbonate solution (95: 5) and supply the weight that subtracts mistake, shake up, filter with microporous filter membrane (0.45um), promptly.
4.4 the investigation precision of linear relationship is measured reference substance solution 2uL, 6uL, 10uL, 14uL, 18uL, sample introduction successively under above-mentioned chromatographic condition, with sample size (ug) is abscissa, peak area (A) carries out linear regression for vertical coordinate, getting the total ferulic acid regression equation is Y=5000000X-22495, r=0.9999, and the result shows, in the 0.053-0.478ug scope, good linear relationship is arranged.
Measure reference substance solution 4.5 precision is investigated precision, press above-mentioned chromatographic condition continuous sample introduction 5 times, each 10uL, the RSD that tries to achieve ferulic acid peak area integrated value is 0.38%, shows that the precision of instrument is good.
Table 4.1 precision is investigated
4.6 replica test
Get with a collection of CHUANSHAO medical material, handle five duplicate samples respectively by the preparation method of need testing solution, sample introduction successively, each 10uL, the RSD that records total ferulic acid is 1.25%, shows that repeatability is better.
Table 4.2 repeatability is investigated (mg/g)
4.7 the recovery test precision takes by weighing 6 parts of 0.25g of same a collection of Rhizoma Chuanxiong medical material of known content, the accurate respectively ferulic acid reference substance that adds is an amount of, handles according to the preparation method of need testing solution, analyzes by above-mentioned chromatographic condition sample introduction, calculates average recovery rate, sees Table 5.3.
Table 4.3 average recovery test (mg/g)
4.8 sample determination is got 5 batches of Rhizoma Chuanxiong medical materials, operates by the preparation method of need testing solution, 3 parts of each sample extraction get testing sample solution.Sampling volume is 10uL, measures peak area, brings regression equation calculation content into, gets 3 results' meansigma methods, the results are shown in following table.
5 batch samples are measured (%)
The method of quality control of Rhizoma Chuanxiong medical material in the concrete embodiment 5 YIXINSHU Chinese medicine preparation
The place of production of Rhizoma Chuanxiong is: the area, Sichuan.
The collection phase of Rhizoma Chuanxiong is: annual excavates in 8-9 month.
The collection processing method of Rhizoma Chuanxiong is: the bright Rhizoma Chuanxiong that takes, remove earth, and Ex-all stem and leaf and fibrous root are soaked in water, and solarization is dried in the air, chip drying behind the moistening.
The discrimination method of Rhizoma Chuanxiong is: get this product content 20g, add ethyl acetate 60ml, reflux, extract, 30min filters, and filtrate is used 5%NaHNO
3Solution extraction 3 times merges the aqueous alkali layer, is acidified to pH1 with dilute sulfuric acid, with extracted with diethyl ether 3 times, combined ether layer, is recycled to driedly, adds methanol 1m and makes dissolving, as need testing solution.Other gets the Rhizoma Chuanxiong control medicinal material and prepares control medicinal material solution as stated above.Get the ferulic acid reference substance more in addition, add methanol and be mixed with the reference substance solution that contains 0.5mg among every 1ml.Draw each 10 μ l of above-mentioned solution respectively, point is on same silica gel G-CMC lamellae, with benzene-ethyl acetate-glacial acetic acid (4: 1: 0.3) is developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
The survey method that contains of Rhizoma Chuanxiong is: the HPLC method is measured content of ferulic acid in the Rhizoma Chuanxiong
Chromatographic condition chromatographic column KromasilC18; Mobile phase: second eyeball: 0.1% glacial acetic acid (18: 82) is a mobile phase; Flow velocity: 1mL/min; Detect wavelength: 320nm; Column temperature: 30 ℃; Theoretical cam curve is calculated by ferulic acid and is not less than 5000.
It is an amount of that the preparation precision of reference substance solution takes by weighing the ferulic acid reference substance, adds methanol one glacial acetic acid (99: 1) and be mixed with the solution that every 1mL contains 26.56ug respectively, shakes up, promptly.
The preparation precision of the need testing solution material powder 0.5g (cross No. 4 sieve) that gets it filled, put in the 50mL tool plug conical flask, accurate methanol one 2% sodium bicarbonate solution (95: the 5) 25mL that adds, ultrasonic 100min, put to room temperature, add methanol one 2% sodium bicarbonate solution (95: 5) and supply the weight that subtracts mistake, shake up, filter with microporous filter membrane (0.45um), promptly.
Accurate respectively above-mentioned reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly.
Content of ferulic acid must not be less than 0.2% in this product.
Claims (4)
1, rhizoma ligustici wallichii quality control method in the YIXINSHU Chinese medicine preparation is characterized in that: it is with the place of production of Rhizoma Chuanxiong, collection, processing, differentiates, contains one of survey project or multinomial index as Rhizoma Chuanxiong quality control in the said preparation.
2, rhizoma ligustici wallichii quality control method in the YIXINSHU Chinese medicine preparation according to claim 1 is characterized in that adopting the part or all of of following method:
(1) place of production of Rhizoma Chuanxiong is: ground such as Sichuan, Yunnan, Guizhou.
(2) acquisition time of Rhizoma Chuanxiong is: annual excavates in 4-10 month.
(3) the collection processing method of Rhizoma Chuanxiong is: the bright Rhizoma Chuanxiong that takes, remove earth, Ex-all stem and leaf and fibrous root, chip drying.
(4) discrimination method of the Radix Astragali is:
Method 1: adopt thin layer chromatography, generally use silica gel G or silica gel G F
254Or silica gel H is a lamellae, the point sample amount is arbitrary volume between 0.5～30 μ l, with the Rhizoma Chuanxiong control medicinal material, ligustrazine, ferulic acid, adenine, adenosine, all or part of kind product in contrast in the vanillin, sample pre-treatments comprises direct sample or with reconcentration method behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, developing solvent can be normal hexane, ethyl acetate, petroleum ether, Ethyl formate, formic acid, dimethylbenzene, toluene, one or more reagent of cyclohexane extraction are formulated according to a certain percentage, and the condition of inspecting comprises under the ultra-violet lamp inspects, put again under the ultra-violet lamp after ammonia is smoked and inspect, or spray is with the chromotropic acid sulfuric acid solution, the anisaldehyde sulfuric acid solution, iodine vapor, the method of 10% phosphomolybdic acid ethanol solution solution colour developing;
Method 2: adopt high performance liquid chromatography or evaporative light scattering detector and high performance liquid chromatography coupling method, sample pre-treatments comprises direct sample or with the method for reconcentration behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, use the chromatographic column of C8 or C18 type filler, with the second eyeball, water, one or more kind solvents in the methanol are mobile phase under the proper ratio condition of routine, with the Rhizoma Chuanxiong control medicinal material, ligustrazine, ferulic acid, adenine, adenosine, all or part of kind product in contrast in the vanillin detect wavelength in 200～600nm scope;
(6) Rhizoma Chuanxiong content adopts following method:
Method 1: adopt high performance liquid chromatography or employing evaporative light scattering detector and high performance liquid chromatography coupling method to measure ligustrazine in this product, ferulic acid, adenine, adenosine, all or part of kind in the vanillin, sample pre-treatments comprises direct sample or with reconcentration method behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, use the chromatographic column of C8 or C18 type filler, with methanol, water, the second eyeball, glacial acetic acid, oxolane, one or more kind solvents in the phosphoric acid solution are mobile phase under the proper ratio condition of routine, detect wavelength in 200～600nm scope;
Method 2: adopt TLC scanning method, generally use silica gel G or silica gel G F
254Or silica gel H is a lamellae, the point sample amount is arbitrary volume between 0.5～30 μ l, with the Rhizoma Chuanxiong control medicinal material, ligustrazine, ferulic acid, adenine, adenosine, all or part of kind product in contrast in the vanillin, sample pre-treatments comprises reconcentration method behind direct sample or ethanol or methanol or water or ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, developing solvent can be chloroform, methanol, ethyl acetate, petroleum ether, Ethyl formate, formic acid, dimethylbenzene, toluene, one or more reagent of cyclohexane extraction are formulated according to a certain percentage, put under the ultra-violet lamp or adopt ammonia smoked after put again and inspect under the ultra-violet lamp or spray method with chromotropic acid sulfuric acid solution or anisaldehyde sulfuric acid solution or iodine vapor or the colour developing of 10% phosphomolybdic acid ethanol solution, speckle adopts single wavelength or dual wavelength to scan on thin-layer chromatogram scanner, and scanning wavelength is 200～400nm;
3, the method for quality control of YIXINSHU astragalus in Chinese medicine preparation according to claim 1 and 2 is characterized in that:
(1) place of production of Rhizoma Chuanxiong is: Sichuan, Yunnan, Guizhou province.
(2) acquisition time of Rhizoma Chuanxiong is: annual excavates in 6-9 month.
(3) the collection processing method of Rhizoma Chuanxiong is: the bright Rhizoma Chuanxiong that takes, remove earth, Ex-all stem and leaf and fibrous root, chip drying behind the moistening that is soaked in water.
(4) discrimination method of Rhizoma Chuanxiong is: adopt thin layer chromatography, use silica gel g thin-layer plate, the point sample amount is an a certain volume between 0.5 μ l～30 μ l, with the product in contrast of all or part of kind in Rhizoma Chuanxiong control medicinal material, the ferulic acid, sample pre-treatments is to use separately or the impurity of mixed solvent extraction according to a certain percentage with chloroform, ether, petroleum ether, use a kind of or dissolved method of they any mixed solvents in ethanol, methanol, ethyl acetate, the water then, developing solvent is normal hexane, ethyl acetate, and the condition of inspecting is that 365nm inspects under the ultra-violet lamp.
(5) Rhizoma Chuanxiong content adopts following method: adopt high performance liquid chromatography or employing evaporative light scattering detector and high performance liquid chromatography coupling method to measure ligustrazine in this product, all or part of kind in the ferulic acid, sample pre-treatments comprises direct sample or with reconcentration method behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, use the chromatographic column of C8 or C18 type filler, with methanol, water, the second eyeball, glacial acetic acid, oxolane, one or more kind solvents in the phosphoric acid solution are mobile phase under the proper ratio condition of routine, detect wavelength in 200～600nm scope;
4, according to rhizoma ligustici wallichii quality control method in the described YIXINSHU Chinese medicine preparation of claim 1～3, it is characterized in that:
(1) place of production of Rhizoma Chuanxiong is: the area, Sichuan.
(2) the collection phase of Rhizoma Chuanxiong is: annual excavates in 8-9 month.
(3) the collection processing method of Rhizoma Chuanxiong is: the bright Rhizoma Chuanxiong that takes, remove earth, and Ex-all stem and leaf and fibrous root are soaked in water, and solarization is dried in the air, chip drying behind the moistening.
(4) discrimination method of Rhizoma Chuanxiong is: get this product content 20g, add ethyl acetate 60ml, reflux, extract, 30min filters, and filtrate is used 5%NaHNO
3Solution extraction 3 times merges the aqueous alkali layer, is acidified to pH1 with dilute sulfuric acid, with extracted with diethyl ether 3 times, combined ether layer, is recycled to driedly, adds methanol 1m and makes dissolving, as need testing solution.Other gets the Rhizoma Chuanxiong control medicinal material and prepares control medicinal material solution as stated above.Get the ferulic acid reference substance more in addition, add methanol and be mixed with the reference substance solution that contains 0.5mg among every 1ml.Draw each 10 μ l of above-mentioned solution respectively, point is on same silica gel G-CMC lamellae, with benzene-ethyl acetate-glacial acetic acid (4: 1: 0.3) is developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
(5) the survey method that contains of Rhizoma Chuanxiong is: the HPLC method is measured content of ferulic acid in the Rhizoma Chuanxiong
Chromatographic condition chromatographic column KromasilC18; Mobile phase: second eyeball: 0.1% glacial acetic acid (18: 82) is a mobile phase; Flow velocity: 1mL/min; Detect wavelength: 320nm; Column temperature: 30 ℃; Theoretical cam curve is calculated by ferulic acid and is not less than 5000.
It is an amount of that the preparation precision of reference substance solution takes by weighing the ferulic acid reference substance, adds methanol one glacial acetic acid (99: 1) and be mixed with the solution that every 1mL contains 26.56ug respectively, shakes up, promptly.
The preparation precision of the need testing solution material powder 0.5g (cross No. 4 sieve) that gets it filled, put in the 50mL tool plug conical flask, accurate methanol one 2% sodium bicarbonate solution (95: the 5) 25mL that adds, ultrasonic 100min, put to room temperature, add methanol one 2% sodium bicarbonate solution (95: 5) and supply the weight that subtracts mistake, shake up, filter with microporous filter membrane (0.45um), promptly.
Accurate respectively above-mentioned reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly.
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