CN103558307A - Detection method of liuwei anxiao preparation - Google Patents
Detection method of liuwei anxiao preparation Download PDFInfo
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- CN103558307A CN103558307A CN201310547674.9A CN201310547674A CN103558307A CN 103558307 A CN103558307 A CN 103558307A CN 201310547674 A CN201310547674 A CN 201310547674A CN 103558307 A CN103558307 A CN 103558307A
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Abstract
The invention discloses a detection method of liuwei anxiao preparation, which overcomes the disadvantages that the detecting operation is complex and the detection result error is large in the prior art. The contents of alantolactone and isoalantolactone in the liuwei xiaoan preparation can be quantitatively detected by a gas chromatographic method, and the specific experiment parameters are obtained through optimization. The detection method has simplicity in operation, high separation degree, strong signal strength, accurate result data, slight human factor influence and strong repeatability.
Description
Technical field
The present invention relates to a kind of detection method of 6-component Anxiao, belong to medical technical field.
Background technology
Existing 6-component Anxiao has Liuwei-Anxiao capsule and Liuwei Anxiao to fall apart; it is the classical proved recipe of Tibetanmedicine; existing more than 100 year history; recording at present the > in < < Chinese Pharmacopoeia >, is the first batch of OTC medicine of national essential drugs, country, national Chinese medicine protection kind.6-component Anxiao is comprised of 6 taste medicines such as Tibet inula root, rheum officinale, Kaempferia galanga, Gypsum (forging), myrobalan, alkali flowers, for having a stomachache turgor, and indigestion, constipation, dysmenorrhoea.
Liuwei-Anxiao capsule and Liuwei Anxiao are loose now carries out < < Chinese Pharmacopoeia > > standard, and rheum officinale is carried out to assay.Document < < HPLC method is measured dissociated anthraquinone in Liuwei-Anxiao capsule, the content > > of general anthraquinone and combined anthraquinone, < < HPLC method is measured anthraquinone component content > > in Liuwei-Anxiao capsule simultaneously, < < HPLC method is measured aloe-emodin in Liuwei-Anxiao capsule simultaneously, Rhein, archen, the content > > of Chrysophanol and Physcion has all introduced distinct methods rheum officinale has been carried out to assay.Document < < GC method is measured three component concentration > > in Liuwei-Anxiao capsule simultaneously and has been introduced a kind of method of simultaneously measuring methoxyl ethyl cinnamate, alantolactone and isoalantolactone, relates to two kinds of medicinal materials of Kaempferia galanga and elecampane (being Tibet inula root).The document adopts GC internal standard method, and chromatographic column is that Dalian Zhong Hui reaches PEG-20M capillary column (30m * 025mm * 025 μ m); Column temperature: 232 ℃, injector temperature: 270 ℃, detector temperature: 260 ℃; Detecting device: FID; Carrier gas: N2; Flow velocity: 45mLmin-1; Sample introduction 1 μ L, split ratio is 5: 1, take ethyl-para-hydroxybenzoate as interior mark.
In 6-component Anxiao, Tibet inula root has strengthening the spleen and stomach, promoting the flow of qi and relieving stagnancy, pain relieving, the drug effect such as antiabortive, is main ingredient in side.In Tibet inula root, contain volatile oil 1%～3%, in oil, principal ingredient is alantolactone and isoalantolactone, modern pharmacology research shows, alantolactone and isoalantolactone have good expelling parasite and antibacterial action, and has excitement and an inhibiting effect to cardiovascular.Therefore be necessary Tibet inula root in Liuwei Anxiao quantitatively to detect.Although document < < GC method is measured three component concentration > > in Liuwei-Anxiao capsule and has been measured three kinds of compositions that comprise alantolactone and isoalantolactone simultaneously simultaneously, but the document is used internal standard method to measure, complicated operation, error is large; Accompanying drawing in document (seeing Fig. 1 of accompanying drawing) can find out, main peak b, c and impurity peaks degree of separation are not ideal, and signal compared with weak and background noise impact obviously.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of detection method of 6-component Anxiao.Technical scheme of the present invention is as follows:
A detection method for 6-component Anxiao, realizes by the content of alantolactone and isoalantolactone in employing vapor-phase chromatography quantitative measurement 6-component Anxiao, and concrete detection method is as follows:
A) chromatographic condition and system suitability: 50% phenyl and 50% dimethyl polysiloxane are the fixing DM-17 capillary column of phase, 30m * 0.25mm * 0.25 μ m, 240 ℃ of column temperatures, 260 ℃ of injector temperatures, 250 ℃ of detector temperatures, detecting device is FID, carrier gas is N
2, number of theoretical plate calculates and is not less than 12000 by alantolactone;
B) preparation of reference substance solution: precision takes alantolactone and isoalantolactone reference substance, adds ethyl acetate and makes respectively every 1ml containing the reference substance solution of alantolactone, each 1mg of isoalantolactone, obtains;
C) preparation of need testing solution: get 6-component Anxiao powder 1-3g, accurately weighed, put in round-bottomed flask, add ethyl acetate 25ml, ultrasonic extraction 1 hour, filter, with 5-15ml ethyl acetate cleaning residue, merging filtrate, is concentrated into dry, with 1-3ml ethyl acetate, be transferred in 5ml measuring bottle and be diluted to scale, obtaining;
D) determination method: precision is drawn reference substance solution and each 2 μ l of need testing solution respectively, and inject gas chromatograph, measures, and obtains.
The unit corresponding relation of weight portion of the present invention and parts by volume is g/ml or kg/l.
6-component Anxiao of the present invention refers to that getting loose bulk drug Tibet inula root 50 weight portions of Liuwei Anxiao, rheum officinale 200 weight portions, Kaempferia galanga 100 weight portions, Gypsum (forging) 250 weight portions, myrobalan's 150 weight portions, alkali spends 300 weight portions, press pharmaceutical formulations common process, add conventional pharmaceutic adjuvant to be prepared into clinical acceptable any peroral dosage form, comprise micropill, dripping pill, tablet, capsule, particle, medicine materical crude slice or dispersing tablet.
Liuwei Anxiao is loose is the nomenclature of drug that < < Chinese Pharmacopoeia > > records.
Beneficial effect: practical operation is found, use the loose middle alantolactone of gas chromatography determination Liuwei Anxiao of Introduction of Literatures and the content of isoalantolactone, complex operation, gained collection of illustrative plates signal to noise ratio (S/N ratio) are not high, and ground unrest impact is larger, and the separating effect of two kinds of compositions is also not ideal.Experimental session chances on, using 50% phenyl and 50% dimethyl polysiloxane is that fixedly the DM-17 capillary column of phase (30m * 0.25mm * 0.25 μ m) can make experiment obtain good separating effect, on this basis, experimenter, through great many of experiments, optimizes and has obtained concrete experiment parameter.Method acquired results data of the present invention are accurately, repeatability is strong, simultaneously easy and simple to handle, degree of separation compared with high, signal intensity is large.
Accompanying drawing explanation
Fig. 1 is the gas chromatogram of the disclosed use internal mark method determination of document methoxyl ethyl cinnamate, alantolactone and isoalantolactone;
Fig. 2 is that alantolactone mixes reference substance solution gas chromatogram with isoalantolactone;
Fig. 3 is the loose need testing solution gas chromatogram of Liuwei Anxiao;
Fig. 4 is negative control solution gas chromatogram;
Fig. 5 is alantolactone linear relationship chart;
Fig. 6 is isoalantolactone linear relationship chart;
Wherein, the horizontal ordinate of Fig. 2, Fig. 3, Fig. 4 is the time, unit: minute (Minutes); Ordinate is voltage, unit: volt (Volts);
The horizontal ordinate of Fig. 5, Fig. 6 is concentration, unit: μ g/ml; Ordinate is peak area, unit: A.
Specific implementation method
Experimental example 1: the assay experiment of alantolactone and isoalantolactone
1. instrument, reagent and test sample
Instrument: Shimadzu GC-2014C gas chromatograph; Shimadzu AUW220D electronic balance.
Reference substance: alantolactone reference substance (Nat'l Pharmaceutical & Biological Products Control Institute, lot number: 110760-200507)
Isoalantolactone reference substance (Nat'l Pharmaceutical & Biological Products Control Institute, lot number: 110761-200204)
Sample: Liuwei Anxiao is loose, and (Qinghai gold is scolded Tibetan medicine medicine company incorporated company and provided, lot number: 20111111,20111112,20111113).
2. system suitability
Under above-mentioned chromatographic condition, precision is drawn blank solvent, reference substance solution, need testing solution, each 1 μ l of negative control solution respectively, and injection liquid chromatography, records chromatogram.Result shows, the degree of separation that in test sample chromatogram, alantolactone and isoalantolactone are adjacent chromatographic peak is all greater than 1.5.Fig. 2 is that alantolactone mixes reference substance solution gas chromatogram with isoalantolactone; Fig. 3 is the loose need testing solution gas chromatogram of Liuwei Anxiao; Fig. 4 is negative control solution gas chromatogram.
3. need testing solution preparation
The investigation of 3.1 extracting method
By method under assay item, need testing solution is detected.By the method under the preparation of need testing solution, prepare 3 parts, ultrasonic, backflow, Zhen Oscillating processes 1 hour respectively.Take in every gram of sample alantolactone and isoalantolactone content determines extracting method as index.The results are shown in Table 1.
Table 1 extracting method is investigated test findings
Result shows, in ultrasonic and every gram of sample of refluxing extraction gained, alantolactone and isoalantolactone content are basically identical, consider that ultrasonic extraction is easy, easy to operate, therefore select extracting method, are ultrasonic extraction.
3.2 extract the investigation of solvent
By method under assay item, need testing solution is detected.By the method under the preparation of need testing solution, prepare 4 parts, precision adds methyl alcohol, ethanol, ethyl acetate, each 25ml of chloroform respectively.Take in every gram of sample alantolactone and isoalantolactone content is that index is determined and extracted solvent.The results are shown in Table 2.
Table 2 extracts solvent and investigates test findings
Result shows, the alantolactone that ethyl acetate extracts and isoalantolactone content are apparently higher than other solvents, and test sample is clean, and degree of separation is good, therefore select, to extract solvent be ethyl acetate.
The investigation of 3.3 extraction times
By method under assay item, need testing solution is detected.By the method under the preparation of need testing solution, prepare 4 parts, ultrasonic processing is 30 minutes, 60 minutes, 90 minutes, 120 minutes respectively.Take in every gram of sample alantolactone and isoalantolactone content determines extraction time as index.The results are shown in Table 3.
Table 3 extraction time investigation test findings chemical drug
Result shows, ultrasonic extraction after 60 minutes in every gram of sample of gained alantolactone and isoalantolactone content basically identical, therefore select extraction time, be 60 minutes.
4. the preparation of typical curve and the investigation of linear relationship
Precision measures alantolactone and isoalantolactone reference substance stock solution solution (alantolactone and isoalantolactone content are respectively 2.1236mg/ml, 2.2456mg/ml) 1ml, 3ml, 5ml, 8ml, 10ml, put respectively in 10ml volumetric flask, with ethyl acetate, be diluted to scale, shake up, each accurate sample introduction 2 μ l, with peak area (A), reference substance concentration (C) is carried out to linear regression, obtain alantolactone and isoalantolactone regression equation: A=114.6C-774.3, A=129.1C+2588, related coefficient: R=0.9999, R=0.9995.Result shows, alantolactone and isoalantolactone are respectively within the scope of 212.36 μ g/ml～2123.60 μ g/ml, 224.56～2245.60 μ g/ml, and the peak area of alantolactone and isoalantolactone (A) is good with reference substance concentration (C) linear relationship.The results are shown in Table 4,5 and Figure of description 5 and Fig. 6.Fig. 5 is alantolactone linear relationship chart; Fig. 6 is isoalantolactone linear relationship chart.
Table 4 alantolactone linear relationship is investigated result
Table 5 isoalantolactone linear relationship is investigated result
5. precision test
Accurate alantolactone and the isoalantolactone reference substance solution 10 μ l of drawing, injection liquid chromatography, each METHOD FOR CONTINUOUS DETERMINATION 6 times, records peak area and calculates relative standard deviation.Result shows, instrument precision is good.The results are shown in Table 6,7.
Table 6 alantolactone Precision test result
Table 7 isoalantolactone Precision test result
6. serviceability test
After prepared by need testing solution, the accurate 10 μ l that draw, injection liquid chromatography, records peak area, measures once every 2 hours later, investigates 8 hours, records peak area and calculates relative standard deviation, is respectively RSD%=1.02%, 0.961%.Result shows, in need testing solution, alantolactone and isoalantolactone measurement result in 8 hours is stable.
7. replica test
Get with the loose sample (product batch number: 20111111) of a collection of Liuwei Anxiao, accurately weighed, totally 6 parts, by the method under the preparation of need testing solution, prepare need testing solution, precision is drawn 10 μ l, injection liquid chromatography, alantolactone and isoalantolactone content in calculation sample respectively, and calculate relative standard deviation, RSD%=1.01%.Result shows, this analytical approach repeatability is good.
8. recovery test
Precision takes with the loose sample (product batch number: 20111111) 6 parts, precision adds alantolactone and isoalantolactone reference substance, measures its content, and calculate recovery rate is 98.2%, RSD%=1.14% of a collection of Liuwei Anxiao.Result shows, this assay method measurement result is accurate.
9. sample determination
Get loose three batches of Liuwei Anxiao, measure and calculate alantolactone and isoalantolactone content.The results are shown in Table 8.
Alantolactone and isoalantolactone assay result in table 8 sample
Embodiment 1: the detection that Liuwei Anxiao is loose
According to complexion spectrometry (appendix VI E of < < Chinese Pharmacopoeia > > version in 2010), measure;
Instrument: Shimadzu GC-2014C gas chromatograph; Shimadzu AUW220D electronic balance.
Reference substance: alantolactone reference substance (Nat'l Pharmaceutical & Biological Products Control Institute, lot number: 110760-200507)
Isoalantolactone reference substance (Nat'l Pharmaceutical & Biological Products Control Institute, lot number: 110761-200204)
Sample: Liuwei Anxiao is loose, and (Qinghai gold is scolded Tibetan medicine medicine company incorporated company and provided, lot number: 20111111,20111112,20111113).
Chromatographic condition and system suitability: 50% phenyl and 50% dimethyl polysiloxane are the fixing DM-17 capillary column of phase (30m * 0.25mm * 0.25 μ m), 240 ℃ of column temperatures, 260 ℃ of injector temperatures, 250 ℃ of detector temperatures, detecting device is FID, carrier gas is N
2, number of theoretical plate calculates and is not less than 12000 by alantolactone;
The preparation of reference substance solution: precision takes alantolactone and isoalantolactone reference substance is appropriate, adds ethyl acetate and makes respectively every 1ml containing the reference substance solution of alantolactone, isoalantolactone 1mg, obtains.
The preparation of need testing solution: get Liuwei Anxiao divided powder 1g, accurately weighed, put in round-bottomed flask, add ethyl acetate 25ml, ultrasonic extraction 1 hour, filter, with 5-15ml ethyl acetate cleaning residue, merging filtrate, be concentrated into dry, with 1-3ml ethyl acetate, be transferred in 5ml measuring bottle, with ethyl acetate, be diluted to scale, obtain.
Determination method: precision is drawn reference substance solution and each 2 μ l of need testing solution respectively, and inject gas chromatograph, measures, and obtains.
This product alantolactone and isoalantolactone content are 0.722mg/g.
Embodiment 2: Liuwei-Anxiao capsule detects
According to complexion spectrometry (appendix VI E of < < Chinese Pharmacopoeia > > version in 2010), measure;
Instrument: Shimadzu GC-2014C gas chromatograph; Shimadzu AUW220D electronic balance.
Reference substance: alantolactone reference substance (Nat'l Pharmaceutical & Biological Products Control Institute, lot number: 110760-200507)
Isoalantolactone reference substance (Nat'l Pharmaceutical & Biological Products Control Institute, lot number: 110761-200204)
Sample: Liuwei-Anxiao capsule is (according to < < Chinese Pharmacopoeia > > self-control, lot number: 20120521,20120522,20120523).
Chromatographic condition and system suitability: 50% phenyl and 50% dimethyl polysiloxane are the fixing DM-17 capillary column of phase (30m * 0.25mm * 0.25 μ m), 240 ℃ of column temperatures, 260 ℃ of injector temperatures, 250 ℃ of detector temperatures, detecting device is FID, carrier gas is N
2, number of theoretical plate calculates and is not less than 12000 by alantolactone;
The preparation of reference substance solution: precision takes alantolactone and isoalantolactone reference substance is appropriate, adds ethyl acetate and makes respectively every 1ml containing the reference substance solution of alantolactone, isoalantolactone 1mg, obtains.
The preparation of need testing solution: get Liuwei-Anxiao capsule content powder 3g, accurately weighed, put in round-bottomed flask, add ethyl acetate 25ml, ultrasonic extraction 1 hour, filter, with 5-15ml ethyl acetate cleaning residue, merging filtrate, be concentrated into dry, with 1-3ml ethyl acetate, be transferred in 5ml measuring bottle, with ethyl acetate, be diluted to scale, obtain.
Determination method: precision is drawn reference substance solution and each 2 μ l of need testing solution respectively, and inject gas chromatograph, measures, and obtains.
This product alantolactone and isoalantolactone content are 0.793mg/g.
Described Liuwei-Anxiao capsule refers to the loose bulk drug formula of Liuwei Anxiao Tibet inula root 50g, rheum officinale 200g, Kaempferia galanga 100g, Gypsum (forging) 250g, myrobalan 150g, alkali flower 300g, by < < Chinese Pharmacopoeia > >, is prepared from.
Embodiment 3: six component medicine detects
According to complexion spectrometry (appendix VI E of < < Chinese Pharmacopoeia > > version in 2010), measure;
Instrument: Shimadzu GC-2014C gas chromatograph; Shimadzu AUW220D electronic balance.
Reference substance: alantolactone reference substance (Nat'l Pharmaceutical & Biological Products Control Institute, lot number: 110760-200507)
Isoalantolactone reference substance (Nat'l Pharmaceutical & Biological Products Control Institute, lot number: 110761-200204)
Sample: six component medicine (self-control, lot number: 20120601,20120602,20120603).
Chromatographic condition and system suitability: 50% phenyl and 50% dimethyl polysiloxane are the fixing DM-17 capillary column of phase (30m * 0.25mm * 0.25 μ m), 240 ℃ of column temperatures, 260 ℃ of injector temperatures, 250 ℃ of detector temperatures, detecting device is FID, carrier gas is N
2, number of theoretical plate calculates and is not less than 12000 by alantolactone;
The preparation of reference substance solution: precision takes alantolactone and isoalantolactone reference substance is appropriate, adds ethyl acetate and makes respectively every 1ml containing the reference substance solution of alantolactone, isoalantolactone 1mg, obtains.
The preparation of need testing solution: get powder 3g after six component medicine porphyrize, accurately weighed, put in round-bottomed flask, add ethyl acetate 25ml, ultrasonic extraction 1 hour, filter, with 5-15ml ethyl acetate cleaning residue, merging filtrate, be concentrated into dry, with 1-3ml ethyl acetate, be transferred in 5ml measuring bottle, with ethyl acetate, be diluted to scale, obtain.
Determination method: precision is drawn reference substance solution and each 2 μ l of need testing solution respectively, and inject gas chromatograph, measures, and obtains.
This product alantolactone and isoalantolactone content are 0.634mg/g.
Described six component medicine refers to the loose bulk drug formula of Liuwei Anxiao Tibet inula root 50g, rheum officinale 200g, Kaempferia galanga 100g, Gypsum (forging) 250g, myrobalan 150g, alkali flower 300g, after simple alcohol extracting and water extraction, medicinal extract adds the conventional pharmaceutic adjuvants such as dextrin, microcrystalline cellulose, talcum powder to be prepared from.
Claims (2)
1. a detection method for 6-component Anxiao, is characterized in that, by the content of alantolactone and isoalantolactone in employing vapor-phase chromatography quantitative measurement 6-component Anxiao, realizes, and concrete detection method is as follows:
A). chromatographic condition and system suitability: 50% phenyl and 50% dimethyl polysiloxane are the fixing DM-17 capillary column of phase, 30m * 0.25mm * 0.25 μ m, 240 ℃ of column temperatures, 260 ℃ of injector temperatures, 250 ℃ of detector temperatures, detecting device is FID, and carrier gas is N
2, number of theoretical plate calculates and is not less than 12000 by alantolactone;
B). the preparation of reference substance solution: precision takes alantolactone and isoalantolactone reference substance, add ethyl acetate and make respectively every 1ml containing the reference substance solution of alantolactone, each 1mg of isoalantolactone, obtain;
C). the preparation of need testing solution: get 6-component Anxiao powder 1-3g, accurately weighed, put in round-bottomed flask, add ethyl acetate 25ml, ultrasonic extraction 1 hour, filter, with 5-15ml ethyl acetate cleaning residue, merging filtrate, is concentrated into dry, with 1-3ml ethyl acetate, be transferred in 5ml measuring bottle and be diluted to scale, obtaining;
D). determination method: precision is drawn reference substance solution and each 2 μ l of need testing solution respectively, and inject gas chromatograph, measures, and obtains.
The composition of described 6-component Anxiao bulk drug and weight portion are: Tibet inula root 50 weight portions, rheum officinale 200 weight portions, kaempferia galamga 100 weight portions, Gypsum (forging) 250 weight portions, myrobalan's 150 weight portions, alkali are spent 300 weight portions.
2. the detection method of 6-component Anxiao according to claim 1, it is characterized in that, described 6-component Anxiao is by pharmaceutical formulations common process, adds conventional pharmaceutic adjuvant to be prepared into clinical acceptable micropill, dripping pill, tablet, capsule, particle, medicine materical crude slice or dispersing tablet peroral dosage form.
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| JPH05148158A (en) * | 1991-11-27 | 1993-06-15 | Sekisui Chem Co Ltd | Promoter for epithelial cell layer permeation of medicine and percutaneous absorption pharmaceutical |
| CN1843396A (en) * | 2006-02-13 | 2006-10-11 | 浙江大德药业集团有限公司 | Oral disintegration tablet for treating coronary heart disease, its preparation process and quality control method |
| CN102526574A (en) * | 2011-12-28 | 2012-07-04 | 江西青春康源制药有限公司 | Traditional Chinese medicine preparation-Liuwei Anxiao Pills and preparing method thereof |
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Application publication date: 20140205 |