CN1487293A - Measuring method of zedoary oil and borneol content in suppository - Google Patents
Measuring method of zedoary oil and borneol content in suppository Download PDFInfo
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- CN1487293A CN1487293A CNA031785018A CN03178501A CN1487293A CN 1487293 A CN1487293 A CN 1487293A CN A031785018 A CNA031785018 A CN A031785018A CN 03178501 A CN03178501 A CN 03178501A CN 1487293 A CN1487293 A CN 1487293A
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- ethyl acetate
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Abstract
The gas chromatographic method is used in measuring the zedoary oil and borneol content in suppository. The measurement method has powerful specialization, good separation effect, high linearity, high stability and high repeatability, and may be used in controlling the quality of the suppository effectively.
Description
[technical field]
The present invention relates to the assay method of drug ingredient.
[background technology]
Baofukang suppository is the kind of recording of one one of Chinese Pharmacopoeia version in 2000, its principal ingredient is oil of zedoary turmeric and borneol, be volatile ingredient, adopt the content of the determination of volatile oil method mensuration oil of zedoary turmeric of steam distillation in the pharmacopeia, this method specificity is not strong, when measuring, mutual interference phenomenon is arranged, and do not stipulate the assay of another principal ingredient borneol in this suppository standard.This product is a Chinese medicine preparation, and composition is complicated, and content assaying method in the past can not control effectively to its main effective constituent.
[summary of the invention]
The objective of the invention is to find a kind of oil of zedoary turmeric in the suppository and borneol are carried out the method for separation determination, measure the content of oil of zedoary turmeric and borneol in the suppository, its effective constituent is carried out effective monitoring.
Purpose of the present invention can be realized by following proposal:
Differentiate: in the collection of illustrative plates that writes down under the content of bornyl alcohol item, the test sample chromatogram should present the chromatographic peak identical with the reference substance chromatographic retention.
The assay photograph vapor-phase chromatography of oil of zedoary turmeric and borneol " an appendix VI of Chinese pharmacopoeia version in 2000 E).
Vapor-phase chromatography:
The moving phase of vapor-phase chromatography is gas, is called carrier gas; Chromatographic column be divided into packed column with two kinds of capillary columns, dress adsorbent in the packed column, porous polymer beads can be coated with the carrier of immobile liquid.The crosslinked immobile liquid of capillary column inwall or carrier.The test sample that injects injection port is heated gasification, and is brought into chromatographic column by carrier gas, in post each composition separated after, successively enter detecting device, chromatographic signal is with registering instrument or data processor processes record.
1, the general requirement of instrument
Used instrument is a gas chromatograph.Except as otherwise herein provided, carrier gas is a nitrogen; Chromatographic column is packed column or capillary column, and the material of packed column is stainless steel or glass, and the carrier diameter is 0.25～0.18 millimeter, 0.18～0.15 millimeter or 0.15～0.125 millimeter zeyssatite or porous polymer beads through pickling and silanization processing; The internal diameter of glass commonly used or fused-silica capillary column is 0.2 millimeter or 0.3 millimeter.Injector temperature should be higher than 30～50 ℃ of column temperatures; Sample size generally is no more than several microlitres; The thin more sample size in post footpath should be few more.Detecting device is a flame ionization ditector, and detected temperatures generally is higher than column temperature, and is not less than 100 ℃, in order to avoid condensation of moisture, general is 250～350 ℃.
2, system suitability test
Stipulate down with the high performance liquid chromatography item.
3, determination method
Stipulate down with the high performance liquid chromatography item.The manual sample size of vapor-phase chromatography is difficult for accurately control, the influence of should notice especially that let the acupuncture needle remain at a certain point time and room temperature.
One, the assay of oil of zedoary turmeric
Chromatographic condition and system suitability test: with polyglycol (PEG)-20M (being Macrogol 2000 0) is the stationary phase capillary column; Column temperature: be 150～200 ℃ of temperature programmes, initial temperature keeps after 10 minutes for 150 ℃, and per minute raises 2 ℃, arrives 180 ℃, keeps after 10 minutes, and per minute raises 10 ℃, and temperature kept 5 minutes for 200 ℃ eventually.Number of theoretical plate calculates by the rcumenol peak should be not less than 10000.
The preparation of reference substance solution: it is an amount of that precision takes by weighing the rcumenol reference substance, adds ethyl acetate and make every milliliter of solution that contains 2.4 milligrams, promptly.
The preparation of need testing solution: get test sample 8.7 grams (5), put in 1000 milliliters of round-bottomed flasks, add 300 milliliters in water, connect volatile oil determination apparatus, add water from the analyzer upper end and make and be full of the scale part, add 3 milliliters of ethyl acetates again, connect reflux condensing tube, reflux 5 hours stops heating, put coldly, divide and to get the ethyl acetate layer, analyzer is again with ethyl acetate washing 3 times, each 5 milliliters, merge ethyl acetate liquid, put in 25 milliliters of measuring bottles, and add ethyl acetate and be diluted to scale, shake up, promptly.
Determination method: accurate respectively reference substance solution and each 1 microlitre of need testing solution drawn, inject gas chromatograph is measured, and calculates, promptly.
Two, the assay of borneol
Chromatographic condition and system suitability test: with polyglycol (PEG)-20M is stationary phase, coating concentration 10%; 130 ℃ of column temperatures.Number of theoretical plate is pressed the naphthalene peak and is calculated, and should be not less than 2400; The degree of separation at borneol, isoborneol peak and naphthalene peak should be up to specification.
Correction factor is measured: it is an amount of to get naphthalene, and accurate the title decides, and adds the ethyl acetate dissolving and makes per 1 milliliter of solution that contains 20 milligrams, shakes up, as inner mark solution.Other gets 75 milligrams of borneol reference substances, and accurate the title decides, and puts in 10 milliliters of measuring bottles, and accurate 2 milliliters of the inner mark solutions that add add the ethyl acetate dissolving and are diluted to scale, shake up, and get 1 microlitre inject gas chromatograph, the calculation correction factor.
The preparation of need testing solution: get test sample 8.7 grams (5), put in 1000 milliliters of round-bottomed flasks, add 300 milliliters in water, connect volatile oil determination apparatus, add water from the analyzer upper end and make and be full of the scale part, add 3 milliliters of ethyl acetates again, connect reflux condensing tube, reflux 5 hours stops heating, puts cold, divide and get the ethyl acetate layer, analyzer with ethyl acetate washing 3 times, each 5 milliliters, merges ethyl acetate liquid again, put in 25 milliliters of measuring bottles, and add ethyl acetate and be diluted to scale, shaking up, precision is measured 5 milliliters, put in 10 milliliters of measuring bottles, accurate 2 milliliters of the inner mark solutions that add add ethyl acetate and are diluted to scale, shake up.
Determination method: draw need testing solution 1 microlitre inject gas chromatograph, measure, promptly.
The content assaying method of oil of zedoary turmeric and borneol in the suppository provided by the invention, the content of oil of zedoary turmeric and borneol in the employing gas chromatography determination suppository, specificity is strong, good separating effect, method linearity, stability, reappearance, recovery test all reach technical requirement preferably, can the quality of suppository be control effectively.
[embodiment]
(1) assay of oil of zedoary turmeric in the Baofukang suppository:
Chromatographic condition and system suitability test: with polyglycol (PEG)-20M is stationary phase, 0.53 mm wide bore capillary column, 1.33 microns of coating film thickness; Column temperature is 150～200 ℃ of temperature programmes, and initial temperature keeps after 10 minutes for 150 ℃, and per minute raises 2 ℃, arrives 180 ℃, keeps after 10 minutes, and per minute raises 10 ℃, and temperature kept 5 minutes for 200 ℃ eventually.Number of theoretical plate calculates by the rcumenol peak should be not less than 10000.
The preparation of reference substance solution: it is an amount of that precision takes by weighing the rcumenol reference substance, adds ethyl acetate and make per 1 milliliter of solution that contains 2.4 milligrams, promptly.
The preparation of need testing solution: get Baofukang suppository 8.7 grams (5), put in 1000 milliliters of round-bottomed flasks, add 300 milliliters in water, connect volatile oil determination apparatus, add water from the analyzer upper end and make and be full of the scale part, add 3 milliliters of ethyl acetates again, connect reflux condensing tube, reflux 5 hours stops heating, put coldly, divide and to get the ethyl acetate layer, analyzer is again with ethyl acetate washing 3 times, each 5 milliliters, merge ethyl acetate liquid, put in 25 milliliters of measuring bottles, and add ethyl acetate and be diluted to scale, shake up, promptly.
Determination method: accurate respectively reference substance solution and each 1 microlitre of need testing solution drawn, inject gas chromatograph is measured, and calculates, promptly.
Every of this product contains oil of zedoary turmeric with rcumenol (C
15H
240
2) meter, must not be less than 10.0 milligrams.
(2) assay of borneol in the Baofukang suppository:
Chromatographic condition and system suitability test: with polyglycol (PEG)-20M is stationary phase, coating concentration 10%; 130 ℃ of column temperatures.Number of theoretical plate is pressed the naphthalene peak and is calculated, and should be not less than 2400; The degree of separation at borneol, isoborneol peak and naphthalene peak should be up to specification.
Correction factor is measured: it is an amount of to get naphthalene, and accurate the title decides, and adds the ethyl acetate dissolving and makes per 1 milliliter of solution that contains 20 milligrams, shakes up, as inner mark solution.Other gets 75 milligrams of borneol reference substances, and accurate the title decides, and puts in 10 milliliters of measuring bottles, and accurate 2 milliliters of the inner mark solutions that add add the ethyl acetate dissolving and are diluted to scale, shake up, and get 1 microlitre inject gas chromatograph, the calculation correction factor.
The preparation of need testing solution: get 5 of Baofukang suppositories, put in 1000 milliliters of round-bottomed flasks, add 300 milliliters in water, connect volatile oil determination apparatus, add water from the analyzer upper end and make and be full of the scale part, add 3 milliliters of ethyl acetates again, connect reflux condensing tube, reflux 5 hours stops heating, puts cold, divide and get the ethyl acetate layer, analyzer with ethyl acetate washing 3 times, each 5 milliliters, merges ethyl acetate liquid again, put in 25 milliliters of measuring bottles, and add ethyl acetate and be diluted to scale, shaking up, precision is measured 5 milliliters, put in 10 milliliters of measuring bottles, accurate 2 milliliters of the inner mark solutions that add add ethyl acetate and are diluted to scale, shake up.
Determination method: draw need testing solution 1 microlitre inject gas chromatograph, measure, promptly.Every of this product contains borneol with borneol (C
10H
18O) and isoborneol (C
10H
18O) total amount meter should be 80.0%～120.0% of labelled amount.
Claims (2)
1. the assay method of oil of zedoary turmeric contents in the suppository is characterized in that
The preparation of reference substance solution: it is an amount of that precision takes by weighing the rcumenol reference substance, adds ethyl acetate and make per 1 milliliter of solution that contains 2.4 milligrams, promptly;
The preparation of need testing solution: get test sample 8.7 grams, put in 1000 milliliters of round-bottomed flasks, add 300 milliliters in water, connect volatile oil determination apparatus, add water from the analyzer upper end and make and be full of the scale part, add 3 milliliters of ethyl acetates again, connect reflux condensing tube, reflux 5 hours stops heating, put coldly, divide and to get the ethyl acetate layer, analyzer washs with ethyl acetate again, merge ethyl acetate liquid, put in 25 milliliters of measuring bottles, and add ethyl acetate and be diluted to scale, shake up, promptly;
Chromatographic condition and system suitability test: with polyglycol (PEG)-20M is the stationary phase capillary column; Column temperature: be 150～200 ℃ of temperature programmes, initial temperature keeps after 10 minutes for 150 ℃, and per minute raises 2 ℃, arrives 180 ℃, keeps after 10 minutes, and per minute raises 10 ℃, and temperature kept 5 minutes for 200 ℃ eventually; Number of theoretical plate calculates by the rcumenol peak should be not less than 10000;
Determination method: accurate respectively reference substance solution and each 1 microlitre of need testing solution drawn, inject gas chromatograph is measured, and calculates, promptly.
2. the assay method of content of bornyl alcohol in the suppository is characterized in that
Correction factor is measured: it is an amount of to get naphthalene, and accurate the title decides, and adds the ethyl acetate dissolving and makes per 1 milliliter of solution that contains 20 milligrams, shakes up, as inner mark solution; Other gets 75 milligrams of borneol reference substances, and accurate the title decides, and puts in 10 milliliters of measuring bottles, and accurate 2 milliliters of the inner mark solutions that add add the ethyl acetate dissolving and are diluted to scale, shake up, and get 1 microlitre inject gas chromatograph, the calculation correction factor;
The preparation of need testing solution: get test sample 8.7 grams, put in 1000 milliliters of round-bottomed flasks, add 300 milliliters in water, connect volatile oil determination apparatus, add water makes and is full of the scale part from analyzer upper end, add 3 milliliters of ethyl acetates again, connect reflux condensing tube, reflux 5 hours, stop heating, put coldly, divide and to get the ethyl acetate layer, analyzer washs with ethyl acetate again, merge ethyl acetate liquid, put in 25 milliliters of measuring bottles, and add ethyl acetate and be diluted to scale, shake up, precision is measured 5 milliliters, put in 10 milliliters of measuring bottles, add ethyl acetate and be diluted to scale, shake up;
Chromatographic condition and system suitability test: with polyglycol (PEG)-20M is stationary phase, coating concentration 10%; 130 ℃ of column temperatures; Number of theoretical plate is pressed the naphthalene peak and is calculated, and should be not less than 2400; The degree of separation at borneol, isoborneol peak and naphthalene peak should be up to specification;
Determination method: draw need testing solution 1 microlitre inject gas chromatograph, measure, promptly.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA031785018A CN1487293A (en) | 2002-07-16 | 2003-07-09 | Measuring method of zedoary oil and borneol content in suppository |
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN02126623.9 | 2002-07-16 | ||
| CN 02126623 CN1415962A (en) | 2002-07-16 | 2002-07-16 | Method for measuring content of oil of zedoary turmeric and borneol in the suppository |
| CNA031785018A CN1487293A (en) | 2002-07-16 | 2003-07-09 | Measuring method of zedoary oil and borneol content in suppository |
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| Publication Number | Publication Date |
|---|---|
| CN1487293A true CN1487293A (en) | 2004-04-07 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA031785018A Pending CN1487293A (en) | 2002-07-16 | 2003-07-09 | Measuring method of zedoary oil and borneol content in suppository |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1322326C (en) * | 2004-12-01 | 2007-06-20 | 天津力神电池股份有限公司 | Method for detecting water content of lithium ion cell electrolyte by gas chromatograply |
| CN101571528B (en) * | 2009-05-18 | 2011-09-21 | 海南碧凯药业有限公司 | Measuring method for oil of zedoary turmeric contents in medicine composition |
| CN102759625A (en) * | 2012-07-26 | 2012-10-31 | 桂林医学院 | Immunoassay application of curcumenol monoclonal antibodies in traditional Chinese medicines including curcumenol |
| CN105158348A (en) * | 2015-06-09 | 2015-12-16 | 湖北荆楚理工科技开发有限公司 | Method for determining five effective components in zedoary oil by using gas chromatography |
| CN116338044A (en) * | 2023-03-17 | 2023-06-27 | 哈尔滨美君制药有限公司 | Quality control method of prescription medicine for Baofukang suppository |
-
2003
- 2003-07-09 CN CNA031785018A patent/CN1487293A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1322326C (en) * | 2004-12-01 | 2007-06-20 | 天津力神电池股份有限公司 | Method for detecting water content of lithium ion cell electrolyte by gas chromatograply |
| CN101571528B (en) * | 2009-05-18 | 2011-09-21 | 海南碧凯药业有限公司 | Measuring method for oil of zedoary turmeric contents in medicine composition |
| CN102759625A (en) * | 2012-07-26 | 2012-10-31 | 桂林医学院 | Immunoassay application of curcumenol monoclonal antibodies in traditional Chinese medicines including curcumenol |
| CN105158348A (en) * | 2015-06-09 | 2015-12-16 | 湖北荆楚理工科技开发有限公司 | Method for determining five effective components in zedoary oil by using gas chromatography |
| CN116338044A (en) * | 2023-03-17 | 2023-06-27 | 哈尔滨美君制药有限公司 | Quality control method of prescription medicine for Baofukang suppository |
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