CN103163240A - Method for quality control of compound aluminic acid bismuth granules - Google Patents
Method for quality control of compound aluminic acid bismuth granules Download PDFInfo
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Abstract
The invention relates to a method for quality control of compound aluminic acid bismuth granules. The method includes a content determination method of emodin in the compound aluminic acid bismuth granules through the adoption of high performance liquid chromatography. The compound aluminic acid bismuth granules comprise frangulae cortex, and each bag of the compound aluminic acid bismuth granules is not less than 0.3mg on the account of the emodin. The prescription ratio of the compound aluminic acid bismuth granules is that 200g of aluminic acid bismuth, 400g of heavy magnesium carbonate, 200g of sodium bicarbonate, 300g of extractum glycyrrhizae, 25g of the frangulae cortex, 10g of fennel powder, and a defined amount of minor ingredients, and 1000 bags are manufactured through mixing, granulation, drying and packaging. The method enables the emodin in the compound aluminic acid bismuth granules to be accurately tested, enables quality of compound aluminic acid bismuth granule drugs to be further effectively controlled, and further guarantees effectiveness and security of the drugs.
Description
Technical field
The present invention relates to the field of quality control of pharmaceutical preparation, particularly, the present invention relates to a kind of method of quality control of compound bismuth aluminate granule.
Background technology
Compound bismuth aluminate granule is a kind of medicine that is used for the treatment of the DDs such as gastric ulcer, duodenal ulcer, chronic superficial gastritis, hyperhydrochloria and duodenal bulbar inflammation, is widely used, and good efficacy and saferry is arranged.Existing national drug standards WS1-(X-047)-2003Z adopts bismuth, aluminium and magnesian content in the titration measuring preparation.Yet the existing drug standards lack the detection method to the Frangula in prescription, can not the content of Frangula be control effectively.Frangula plays an important role in prescription, the effects such as laxative, promotion enterogastric peristalsis are arranged, help to eliminate the constipation that in prescription, other composition causes, help lend some impetus to digestion, eliminate abdominal distension discomfort etc., cooperatively interact with other composition, acting in conjunction, the treatment DD.If lack the control to Frangula content, the content of this important component just can not effective guarantee, makes the validity of medicine and security have hidden danger.
Summary of the invention
The object of the invention is to, a kind of method of quality control of compound bismuth aluminate granule is provided, the method can accurately be measured the contained archen of Frangula in compound bismuth aluminate granule, thereby controls the content of Frangula, has ensured validity and the security of medicine.
In order to achieve the above object, the present invention has adopted following technical scheme:
A kind of method of quality control of compound bismuth aluminate granule, described method comprise the employing high performance liquid chromatography to the content assaying method of archen in compound bismuth aluminate granule, and compound bismuth aluminate granule contains Frangula in archen, and every bag is no less than 0.3mg.
The prescription ratio of described compound bismuth aluminate granule is bismuth aluminate 200g, heavy magnesium carbonate 400g, sodium bicarbonate 200g, extract of licorice root 300g, Frangula 25g, fennel powder 10g, right amount of auxiliary materials, through mixing, granulation, dry, packing, makes 1000 bags.
Described employing high performance liquid chromatography is as follows to the content assaying method of archen in compound bismuth aluminate granule:
Chromatographic condition and system suitability test: take octadecylsilane chemically bonded silica as filling agent, take methyl alcohol: the Volume fraction of 0.1% phosphoric acid solution is as 75～80:25～20 as mobile phase, the detection wavelength is 254～295nm, and number of theoretical plate should be not less than 3000 by archen peak calculating;
The reference substance solution preparation: get the archen reference substance appropriate, accurately weighed, put in dosing container, add methenyl choloride, then add the methyl alcohol dissolving, shake up, make the solution that every 1ml contains archen 5～25 μ g, and get final product;
the preparation of need testing solution: get 10 bags of compound bismuth aluminate granules, accurately weighed every bag of content, with contents mixed, porphyrize, get 0.03～0.75g, accurately weighed, add 6%～10% acid solution 2～50ml, standing 10 minutes, add again methenyl choloride 4～100ml, be heated to boiling hydrolysis 0.5～3.5 hour, hydrolyzate is inserted in separating funnel, tell the methenyl choloride layer, acid solution is extracted 0～5 time with methenyl choloride again, each 4～100ml, merge methenyl choloride liquid, be recycled to dried, residue adds the methyl alcohol dissolving, be transferred in 2～50ml dosing container, add methanol constant volume, shake up, and get final product,
Determination method: precision is drawn reference substance solution and each 5～20 μ L of need testing solution respectively, and the injection liquid chromatography is measured, and be get final product.
The acid solution that uses in the present invention is any in phosphoric acid solution, sulfuric acid solution and hydrochloric acid solution.
According to a preferred embodiment of the invention, a kind of method of quality control of compound bismuth aluminate granule:
Chromatographic condition and system suitability test: take octadecylsilane chemically bonded silica as filling agent, take methyl alcohol: the Volume fraction of 0.1% phosphoric acid solution is as 78:22 as mobile phase, and the detection wavelength is 285nm, and number of theoretical plate calculates by the archen peak should be not less than 3000;
The reference substance solution preparation: get the archen reference substance appropriate, accurately weighed, put in dosing container, add appropriate methenyl choloride, then add the methyl alcohol dissolving, shake up, make the solution that every 1ml contains archen 16 μ g, and get final product;
The preparation of need testing solution: get 10 bags of compound bismuth aluminate granules, accurately weighed every bag of content is with contents mixed, porphyrize, get 0.15g, accurately weighed, add 8% hydrochloric acid solution 10ml, standing 10 minutes, add again methenyl choloride 20ml, be heated to boiling hydrolysis 2 hours, hydrolyzate is inserted in separating funnel, tell the methenyl choloride layer, acid solution is extracted 3 times with methenyl choloride again, and each 20ml merges methenyl choloride liquid, be recycled to dried, residue adds the methyl alcohol dissolving, is transferred in the 10ml dosing container, adds methanol constant volume, shake up, and get final product;
Determination method: precision is drawn reference substance solution and each 10 μ L of need testing solution respectively, and the injection liquid chromatography is measured, and be get final product.
The present invention has following advantage with respect to prior art: the present invention adopts acid hydrolysis to process test sample, and flow phase and detection wavelength are selected, can accurately detect emodin content in preparation, overcome the defective that existing detection method can not detect archen in compound bismuth aluminate granule, thereby solve existing drug standards shortage to the problem of the detection method of Frangula, content to Frangula has carried out effective control, effective guarantee the content of this important component, further ensured validity and the security of this medicine.
Embodiment
The present invention is further detailed explanation with embodiment for the below.
Compound bismuth aluminate granule is by ingredients such as bismuth aluminate, heavy magnesium carbonate, sodium bicarbonate, extract of licorice root, Frangula, fennel powders.For further controlling drug quality, according to ingredients, wherein Frangula contains the anthraquinone glycoside of archen and archen thereof, by prerun, can carry out high-efficient liquid phase technique to its assay.For guaranteeing the quality of preparation, to the condition determination of archen in this product, carried out system test, set up the high efficiency liquid phase determination method, can measure the emodin content in this product.
1, instrument and reagent
Instrument: Shimadzu LC-20AT full automatic high efficiency liquid chromatograph, diode array detector; KQ100 type ultrasonic cleaner (city of Kunshan ultrasonic instrument factory).
Reagent: methyl alcohol is that chromatographically pure, water are the Wahaha pure water, and phosphoric acid, methyl alcohol are that analysis is pure, and it is pure that other reagent are analysis.
Archen reference substance: available from Nat'l Pharmaceutical ﹠ Biological Products Control Institute's (lot number: 110756-200110 assay specification).
The compound bismuth aluminate granule test sample: Liaoning Aoda Pharmaceutical Co., Ltd produces, and lot number is: 20110307.
2, chromatographiccondition
Chromatographic column: filler is: Kromasil-C
18, 5 μ, 4.6 * 250mm (Beijing Analytical Instrument Factory's product).
Column temperature: 30 ℃.
Flow velocity: 1.0ml/min.
Degree of separation (R): archen and adjacent assorted peak degree of separation are greater than 1.5.
Number of theoretical plate: should be not less than 3000 by archen peak calculating.
3, method and result
(1) mobile phase and absorbing wavelength are selected
Press the assay method of archen in document and pharmacopeia, all can't measure the content of archen in compound bismuth aluminate granule, flow phase of the present invention and absorption detecting wavelength have carried out great many of experiments, successively the ratio with methyl alcohol-0.1% phosphoric acid solution changes 80:20 and 78:22 into, 75:25, archen and other peaks can be separated, and the ratio of 78:22 is best.Then select through spectrum again, investigate to the 300nm wavelength from 250nm, successively find 254,275,280,285,290, larger absorption arranged under 295nm equiwavelength, and 285nm wavelength place to this product in the archen peak area maximum, the negative minimum of disturbing, only account for 0.70% of the total area, more meet the requirement that high efficiency liquid phase is measured.Therefore it is mobile phase that the present invention preferably adopts methyl alcohol-0.1% phosphoric acid (78:22), absorbing wavelength is under the condition of 285nm, and archen in Frangula is measured.
(2) linear relationship is investigated
Inject respectively archen reference substance methanol solution (0.01776 μ g/ μ l) 3,6,9,12,15 μ l in chromatograph, measure peak area, take archen sample size (μ g number) as horizontal ordinate, peak area is ordinate, the drawing standard curve, its regression equation is: Y=443696.2X-17946.9, r=0.9999.Result shows, archen has good linear relationship in 0.05328 ~ 0.2664 μ g scope, the results are shown in Table 1.
Table 1 archen linear relationship
(3) hydrolysis acid and acid concentration are selected
Sample thief number part, only adding methenyl choloride 20ml, and after first adding respectively 6%, 8%, 10% hydrochloric acid, phosphoric acid, each 10ml of sulfuric acid, then add under the condition of methenyl choloride 20ml, press emodin content method for measuring hydrolysis, sample preparation, mensuration, the results are shown in Table 2.
Table 2 Different solution extraction comparison result
The above results shows, adopts 6%～10% hydrochloric acid as the hydrolysis solvent, and emodin content is approximate, and wherein, 8% hydrochloric acid result is the highest, therefore test sample preferably adopts 8% hydrochloric acid to be the hydrolysis solvent.
In the research compound bismuth aluminate granule in the process of emodin content assay method, during the preparation need testing solution, if only adopt methenyl choloride to extract, emodin content is very low after measured for the need testing solution of preparation, with get the Frangula of same amount by compound bismuth aluminate granule prescription, the result of measuring that uses the same method differs greatly, so that can not be as the method for quality control.Through test of many times, analysis, after the researchist has paid a large amount of performing creative labours, find to adopt acid-hydrolyzed method can eliminate the defective of above-mentioned detection method, therefore, set up emodin content assay method in compound bismuth aluminate granule.
(4) hydrolysis time is selected test
Sample thief number part adds respectively 8% hydrochloric acid 10ml, methenyl choloride 20ml, by the emodin content method for measuring be hydrolyzed respectively 1 hour, 1.5 hours, 2 hours, sample preparation is measured, and the results are shown in Table 3.
Table 3 Different Extraction Method comparative result
The above results shows, is hydrolyzed 0.5～3.5 hour, and emodin content is more stable, and especially heating hydrolysis is 2 hours and 3.5 hours, and emodin content is higher, considers, adopt 2 hours more economical, therefore test sample adopted hydrolysis time 2 hours.
(5) blank test
Ratio in the prescription taste of traditional Chinese medicine, autogamy does not contain group's medicine of Frangula, make blank preparation by preparation process, make blank solution by the need testing solution preparation method again, measure in accordance with the law, result shows the negative sample that does not contain Frangula, the place has very faint peak to occur in retention time identical with the archen reference substance, its peak area only accounts for 0.7% left and right of test sample peak area, well below below 5%, therefore think substantially noiseless to measuring.
(6) precision test
Precision takes sample, makes need testing solution by the emodin content method for measuring, repeats sample introduction 5 times, measures peak area, the results are shown in Table 4.
Table 4 Precision test result
(7) stability test
Precision takes sample, makes need testing solution by the emodin content assay method, respectively at rear 0,3,6,9,12,24 hour of preparation, measures in accordance with the law, and result shows that need testing solution is basicly stable in 27 hours, the results are shown in Table 5.
Table 5 stability test result
(8) replica test
Press the emodin content method for measuring, to same lot number sample, measure, try to achieve relative standard deviation less than 5%, the results are shown in Table 6.
Table 6 replica test
(9) recovery test
Adopt the application of sample absorption method, accurate absorption archen reference substance methanol solution (0.0606mg/mL) 1ml6 part is put in 1 ~ No. 6 100mL round-bottomed flask of numbering, flings to methyl alcohol in water-bath.The same batch sample of getting again known content is the 75mg left and right approximately, and is accurately weighed, press preparation method's preparation and above-mentioned chromatographic condition that emodin content is measured need testing solution, and mensuration is calculated as follows the recovery, the results are shown in Table 7.
Table 7 archen determination of recovery rates result
(10) sample determination
Press the emodin content assay method, get 11 batch samples and measure in accordance with the law, the results are shown in Table 8.
Table 8 sample determination result
According to above measurement result, every bag of this product contains Frangula with archen (C
15H
10O
5) meter, should be less than 0.3mg.
Embodiment 1
A kind of method of quality control of compound bismuth aluminate granule, described method comprises the content assaying method to archen in compound bismuth aluminate granule.
Compound bismuth aluminate granule prescription ratio is bismuth aluminate 200g, heavy magnesium carbonate 400g, sodium bicarbonate 200g, extract of licorice root 300g, Frangula 25g, fennel powder 10g, auxiliary material hydroxypropyl cellulose 165g, after mixing, with 75% ethanol wet granulation, drying, pack by the specification of every bag of 1.3g, make approximately 1000 bags.
Chromatographic condition and system suitability test: take octadecylsilane chemically bonded silica as filling agent, take methyl alcohol: the Volume fraction of 0.1% phosphoric acid solution is as 78:22 as mobile phase, and the detection wavelength is 285nm, and number of theoretical plate calculates by the archen peak should be not less than 3000;
The reference substance solution preparation: get the archen reference substance appropriate, accurately weighed, put in the 25ml measuring bottle, add the 5ml methenyl choloride, then add methyl alcohol to scale, ultrasonic dissolution shakes up, and makes the mother liquor that every 1ml contains archen 80 μ g.Draw in this solution 2ml to 10ml measuring bottle, add methyl alcohol to scale, shake up, make the solution that every 1ml contains archen 16 μ g, and get final product;
the preparation of need testing solution: get 10 bags of compound bismuth aluminate granules, accurately weighed every bag of content, with contents mixed, porphyrize, get 0.15g, accurately weighed, add 8% hydrochloric acid solution 10ml, standing 10 minutes, add again methenyl choloride 20ml, put in the electric jacket that has heated, first heat 5 minutes to boiling, continued again heating hydrolysis 2 hours, take off, place slightly cold, hydrolyzate is inserted in separating funnel, tell the methenyl choloride layer, acid solution is extracted 3 times with methenyl choloride again, each 20ml, tell the methenyl choloride layer and merge, reclaim methenyl choloride to doing, residue adds the methyl alcohol dissolving, be transferred in the 10ml measuring bottle, add methyl alcohol to scale, shake up, and get final product,
Determination method: precision is drawn reference substance solution and each 10 μ L of need testing solution respectively, and the injection liquid chromatography is measured, and as calculated, every bag contains Frangula with archen (C
15H
10O
5) meter, average out to 0.598mg.
Embodiment 2
A kind of method of quality control of compound bismuth aluminate granule, described method comprises the content assaying method to archen in compound bismuth aluminate granule.
Compound bismuth aluminate granule prescription ratio is bismuth aluminate 200g, heavy magnesium carbonate 400g, sodium bicarbonate 200g, extract of licorice root 300g, Frangula 25g, fennel powder 10g, auxiliary material hydroxypropyl cellulose 165g, after mixing, with 75% ethanol wet granulation, drying, pack by the specification of every bag of 1.3g, make approximately 1000 bags.
Chromatographic condition and system suitability test: take octadecylsilane chemically bonded silica as filling agent, take ethanol: the Volume fraction of 0.1% phosphoric acid solution is as 75:25 as mobile phase, and the detection wavelength is 295nm, and number of theoretical plate calculates by the archen peak should be not less than 3000;
The reference substance solution preparation: get the archen reference substance appropriate, accurately weighed, put in dosing container, add the 5ml methenyl choloride, then add the methyl alcohol dissolving, shake up, make the solution that every 1ml contains archen 5 μ g, and get final product;
The preparation of need testing solution: get 10 bags of compound bismuth aluminate granules, accurately weighed every bag of content is with contents mixed, porphyrize is got 0.03g, porphyrize, accurately weighed, add 6% sulfuric acid solution 2ml, standing 10 minutes, then add methenyl choloride 4ml, be heated to boiling hydrolysis 0.5 hour, hydrolyzate is inserted in separating funnel, tell the methenyl choloride layer, acid solution is extracted 5 times with methenyl choloride again, each 4ml, tell the methenyl choloride layer and merge, being recycled to driedly, residue adds the ethanol dissolving, be transferred in the 2ml dosing container, add methanol constant volume, shake up, and get final product;
Determination method: precision is drawn reference substance solution and each 20 μ L of need testing solution respectively, and the injection liquid chromatography is measured, and as calculated, every bag contains Frangula with archen (C
15H
10O
5) meter, average out to 0.352mg.
Embodiment 3
A kind of method of quality control of compound bismuth aluminate granule, described method comprises the content assaying method to archen in compound bismuth aluminate granule.
Compound bismuth aluminate granule prescription ratio is bismuth aluminate 200g, heavy magnesium carbonate 400g, sodium bicarbonate 200g, extract of licorice root 300g, Frangula 25g, fennel powder 10g, auxiliary material hydroxypropyl cellulose 165g, after mixing, with 75% ethanol wet granulation, drying, pack by the specification of every bag of 1.3g, make approximately 1000 bags.
Chromatographic condition and system suitability test: take octadecylsilane chemically bonded silica as filling agent, take methyl alcohol: the Volume fraction of 0.1% phosphoric acid solution is as 80:20 as mobile phase, and the detection wavelength is 254nm, and number of theoretical plate calculates by the archen peak should be not less than 3000;
The reference substance solution preparation: get the archen reference substance appropriate, accurately weighed, put in dosing container, add the 5ml methenyl choloride, then add the methyl alcohol dissolving, shake up, make the solution that every 1ml contains archen 25 μ g, and get final product;
The preparation of need testing solution: get 10 bags of compound bismuth aluminate granules, accurately weighed every bag of content, with contents mixed, porphyrize, get 0.75g, porphyrize, accurately weighed, add 10% phosphoric acid solution 50ml, standing 10 minutes, then add methenyl choloride 100ml, be heated to boiling hydrolysis 3.5 hours, hydrolyzate is inserted in separating funnel, tell the methenyl choloride layer, be recycled to driedly, residue adds methyl alcohol dissolving, is transferred in the 50ml dosing container, add methanol constant volume, shake up, and get final product;
Determination method: precision is drawn reference substance solution and each 5 μ L of need testing solution respectively, and the injection liquid chromatography is measured, and as calculated, every bag contains Frangula with archen (C
15H
10O
5) meter, average out to 0.344mg.
Claims (5)
1. the method for quality control of a compound bismuth aluminate granule, described method comprise and adopt high performance liquid chromatography to the content assaying method of archen in compound bismuth aluminate granule, and compound bismuth aluminate granule contains Frangula in archen, and every bag is no less than 0.3mg.
2. the method for quality control of compound bismuth aluminate granule as claimed in claim 1, it is characterized in that, the prescription ratio of described compound bismuth aluminate granule is bismuth aluminate 200g, heavy magnesium carbonate 400g, sodium bicarbonate 200g, extract of licorice root 300g, Frangula 25g, fennel powder 10g, right amount of auxiliary materials, through mixing, granulation, dry, packing, make 1000 bags.
3. the method for quality control of compound bismuth aluminate granule as claimed in claim 1 or 2, is characterized in that, described employing high performance liquid chromatography is as follows to the content assaying method of archen in compound bismuth aluminate granule:
Chromatographic condition and system suitability test: take octadecylsilane chemically bonded silica as filling agent, take methyl alcohol: the Volume fraction of 0.1% phosphoric acid solution is as 75～80:25～20 as mobile phase, the detection wavelength is 254～295nm, and number of theoretical plate should be not less than 3000 by archen peak calculating;
The reference substance solution preparation: get the archen reference substance appropriate, accurately weighed, put in dosing container, add methenyl choloride, then add the methyl alcohol dissolving, shake up, make the solution that every 1ml contains archen 5～25 μ g, and get final product;
the preparation of need testing solution: get 10 bags of compound bismuth aluminate granules, accurately weighed every bag of content, with contents mixed, porphyrize, get 0.03～0.75g, accurately weighed, add 6%～10% acid solution 2～50ml, standing 10 minutes, add again methenyl choloride 4～100ml, be heated to boiling hydrolysis 0.5～3.5 hour, hydrolyzate is inserted in separating funnel, tell the methenyl choloride layer, acid solution is extracted 0～5 time with methenyl choloride again, each 4～100ml, merge methenyl choloride liquid, be recycled to dried, residue adds the methyl alcohol dissolving, be transferred in 2～50ml dosing container, add methanol constant volume, shake up, and get final product,
Determination method: precision is drawn reference substance solution and each 5～20 μ L of need testing solution respectively, and the injection liquid chromatography is measured, and calculates, and get final product.
4. the method for quality control of compound bismuth aluminate granule as claimed in claim 3, is characterized in that, described acid solution is any in phosphoric acid solution, sulfuric acid solution and hydrochloric acid solution.
5. the method for quality control of compound bismuth aluminate granule as claimed in claim 4, is characterized in that,
Chromatographic condition and system suitability test: take octadecylsilane chemically bonded silica as filling agent, take methyl alcohol: the Volume fraction of 0.1% phosphoric acid solution is as 78:22 as mobile phase, and the detection wavelength is 285nm, and number of theoretical plate calculates by the archen peak should be not less than 3000;
The reference substance solution preparation: get the archen reference substance appropriate, accurately weighed, put in dosing container, add appropriate methenyl choloride, then add the methyl alcohol dissolving, shake up, make the solution that every 1ml contains archen 16 μ g, and get final product;
The preparation of need testing solution: get 10 bags of compound bismuth aluminate granules, accurately weighed every bag of content is with contents mixed, porphyrize, get 0.15g, accurately weighed, add 8% hydrochloric acid solution 10ml, standing 10 minutes, add again methenyl choloride 20ml, be heated to boiling hydrolysis 2 hours, hydrolyzate is inserted in separating funnel, tell the methenyl choloride layer, acid solution is extracted 3 times with methenyl choloride again, and each 20ml merges methenyl choloride liquid, be recycled to dried, residue adds the methyl alcohol dissolving, is transferred in the 10ml dosing container, adds methanol constant volume, shake up, and get final product;
Determination method: precision is drawn reference substance solution and each 10 μ L of need testing solution respectively, and the injection liquid chromatography is measured, and calculates, and get final product.
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| CN1150024A (en) * | 1995-11-13 | 1997-05-21 | 营口市第二制药厂 | Prescription and technique of compound bismuth aluminate granule |
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| US20130000389A1 (en) * | 2011-06-29 | 2013-01-03 | Kaohsiung Medical University | Chemical profile of detecting bioactive components of quinones, stilbenes, flavones and alkaloids |
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2013
- 2013-02-26 CN CN2013100626345A patent/CN103163240A/en active Pending
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| CN1150024A (en) * | 1995-11-13 | 1997-05-21 | 营口市第二制药厂 | Prescription and technique of compound bismuth aluminate granule |
| CN101940635A (en) * | 2010-09-07 | 2011-01-12 | 哈药集团三精千鹤望奎制药有限公司 | Nanometer ceanothus bismuth magnesium tablet and preparation method thereof |
| US20130000389A1 (en) * | 2011-06-29 | 2013-01-03 | Kaohsiung Medical University | Chemical profile of detecting bioactive components of quinones, stilbenes, flavones and alkaloids |
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Application publication date: 20130619 |