CN103293242B - Method for measuring calcium stearate in drug - Google Patents
Method for measuring calcium stearate in drug Download PDFInfo
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- CN103293242B CN103293242B CN201310211968.4A CN201310211968A CN103293242B CN 103293242 B CN103293242 B CN 103293242B CN 201310211968 A CN201310211968 A CN 201310211968A CN 103293242 B CN103293242 B CN 103293242B
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Abstract
The invention belongs to the technical field of analysis chemistry and particularly relates to a method for measuring calcium stearate in a drug. The method comprises the following steps of: 1) extracting a sample solution, adding hydrochloric acid to the sample solution to acidize the sample solution, extracting through normal hexane to obtain a normal hexane extracting solution, rotationally evaporating and concentrating the normal hexane extracting solution, and blowing to dryness by using nitrogen; 2) carrying out methyl esterifying, namely, adding methanol into the solution to dissolve, adding sulfuric acid, uniformly mixing, and extracting a methyl esterified product through normal hexane, helically and uniformly mixing, stewing for layering and extracting the normal hexane layer; 3) measuring the dosage of the methyl stearate in the normal hexane layer obtained in step 2) through a gas chromatograph-mass spectrometer; and 4) finally calculating the content of calcium stearate in the sample solution according to the dosage of the methyl stearate obtained in step 3). The method disclosed by the invention is used for measuring calcium stearate in the drug through the gas chromatograph-mass spectrometer by acidizing the sample to extract stearic acid; and the measuring method is not only quick and simple, but also capable of being used for accurately measuring the content of calcium stearate in the drug, and the detection limit is low.
Description
[technical field]
The invention belongs to technical field of analytical chemistry, specifically a kind of method of measuring calcium stearate in medicine.
[background technology]
In modern medicine packaging, extensively adopt plastic product as medicine package main body, adopt rubber or plastic material to make sealing plug or the pad of medicine bottle.Due to these wrappage and the medicament contact that enters human body, so have strict requirement for drug packing material, only in the chemical property of these packaging materials, will detect extract as adjuvant, monomer residue thing, decomposition/catabolite in material, move in addition thing as the migration of the monomers such as adjuvant, monomer residue thing, decomposition/catabolite, bonding agent, ink.Common adjuvant in plastic package material has modifier, stabilizing agent, colorant, lubricant etc.
Calcium stearate, as stabilizing agent and the lubricant of Polyvinylchloride, can make the nontoxic flexible film such as packaging for foodstuff, medicine equipment vessel.In tygon, polypropylene as halogen-absorber, the lubricant of catalyzer residual in resin to color of resin and moulded work be can eliminate, the release agent of the lubricant of the thermosetting plastics such as phenolic aldehyde, amino and polyester reinforced plastic, intensifier, the water-proofing agent of textile and the flatting agent of paint etc. of railway grease also can be made.
Calcium stearate is widely used in medicine packaging as the lubricant of medical plastic and rubber.In the contact process of medicine packaging and medicine, calcium stearate may move in medicine, cause drug appearance and physicochemical property, the even change of drug effect, thereby directly enter human vas by the absorption of medicine or through injection, drop etc., cause the direct injury to human body.Therefore before medicine comes into the market, not only to investigate the stability of medicine packaging, with the migration of the stability of the medicine of wrappage packaging and the various monomers that caused by medicine packaging material be also the emphasis of consideration.
Calcium stearate has had the report of some relevant test methods as the adjuvant in food additives and plastics.As adopt fourier transform infrared spectroscopy (FTIR) to carry out fast qualitative analysis utilizing to the calcium stearate in atactic copolymerized polypropene (PP-R), the calcium stearate in atactic copolymerized polypropene sample is carried out to preliminary quantitative test.Adopt inductively coupled plasma-atomic emission spectrometry (ICP-AES) indirect determination calcium stearate content etc.Also useful thin layer chromatography detects calcium stearate content.But these methods are qualitative or tentatively quantitative mostly, can not carry out accurate quantitative analysis to calcium stearate.
Calcium stearate is the important indicator of medicine packaging and medicine Study on Compatibility as the pollutant in medicine, and accurate and trace detection is very important.
[summary of the invention]
Object of the present invention is exactly will solve above-mentioned deficiency and provide a kind of acidifying extraction, gas chromatograph-mass spectrometer to measure the method for calcium stearate in medicine, not only assay method is quick, simple, and can realize the Accurate Determining of calcium stearate content in medicine.
Design for achieving the above object a kind of method of measuring calcium stearate in medicine, comprise the following steps:
1) sample pretreatment: extracting sample solution, add hcl acidifying, extract through normal hexane, obtain hexane extract, concentrated hexane extract rotary evaporation and nitrogen are blown to dry;
2) esterification: add methyl alcohol to dissolve, then add sulfuric acid to mix, with normal hexane extraction esterification product, vortex mixes, and stratification is got normal hexane layer;
3) adopt gas chromatograph-mass spectrometer determination step 2) amount of methyl stearate in the normal hexane layer of gained, the condition determination of gas chromatograph-mass spectrometer is: gas chromatographic column adopts HP-5MS capillary column, specification is 30 meters of column lengths, 0.25 millimeter of column internal diameter, 0.25 micron of thickness; Gas chromatographic sample introduction mouth Temperature Setting is 280 DEG C, and temperature programme is 100 DEG C of initial temperature, is warmed up to 300 DEG C by 30 DEG C of per minutes, retains 5 minutes; Ion scan pattern is selected in mass spectrum collection, and scan ion is m/z 74, m/z 87, m/z 298;
4) last, according to step 3) amount of the methyl stearate of gained, the content of calcium stearate in calculation sample solution, wherein, the reduction coefficient of calcium stearate and methyl stearate
Above-mentioned steps 1) in, sample is solution-type medicine or parenteral solution, draws sample solution, add hydrochloric acid, mix, 60 DEG C of ultrasonic acidifyings of water-bath 1 hour, are transferred to sample solution in separating funnel after cooling, add water and mix, divide 3 extractions through normal hexane, hexane extract is crossed to anhydrous sodium sulfate dehydration, 40 DEG C of Rotary Evaporators are concentrated into and are less than 2mL, shift solution to glass centrifuge tube, nitrogen dries up.
Above-mentioned steps 1) in, sample is solid medicine, takes even medicinal powder, add water ultrasonic dissolution sample, obtain sample solution, pipette sample solution in vial, add hydrochloric acid, mix, 60 DEG C of ultrasonic acidifyings of water-bath 1 hour, after cooling sample solution is transferred in separating funnel, adds water and mixes, divide 3 extractions through normal hexane, hexane extract is crossed to anhydrous sodium sulfate dehydration, 40 DEG C of Rotary Evaporators are concentrated into and are less than 2mL, shift solution to glass centrifuge tube, and nitrogen dries up.
The present invention compared with the existing technology, beneficial effect is: the present invention is that stearic acid is extracted in a kind of sample acidifying, gas chromatograph-mass spectrometer is measured the method for calcium stearate in medicine, not only assay method fast, simply, and can realize the Accurate Determining of calcium stearate content in medicine, its detection limit is very low, and having solved traditional method of testing for calcium stearate is qualitative or tentatively quantitative mostly, can not carry out to calcium stearate the problem of accurate quantitative analysis.
[brief description of the drawings]
Fig. 1 is the gas chromatogram of methyl stearate in embodiment 2;
Fig. 2 is the mass spectrogram of methyl stearate in embodiment 2.
[embodiment]
The invention belongs to the mensuration to calcium stearate in medicine in analytical chemistry field, its principle is: by the calcium stearate in drug sample through hcl acidifying, obtain stearic acid, stearic acid obtains methyl stearate through normal hexane extraction and methyl alcohol, Methylsulfate, measured again the amount of methyl stearate by GC/MS gas chromatograph-mass spectrometer, finally, calculated the content of calcium stearate by the amount of methyl stearate, wherein, the reduction coefficient of calcium stearate and methyl stearate
The condition determination of gas chromatograph-mass spectrometer is:
1) gas chromatographic column adopts HP-5MS capillary column, and specification is 30 meters of column lengths, 0.25 millimeter of column internal diameter, 0.25 micron of thickness;
2) gas chromatographic sample introduction mouth Temperature Setting is 280 DEG C, and temperature programme is 100 DEG C of initial temperature, is warmed up to 300 DEG C by 30 DEG C of per minutes, retains 5 minutes;
3) ion scan pattern is selected in mass spectrum collection, and scan ion is m/z 74, m/z 87, m/z 298.
Embodiment 1: the mensuration of calcium stearate in sodium chloride injection
1. the preparation of sample:
Draw sodium chloride injection 4mL, add 400 hydrochloric acid, mix, 60 DEG C of ultrasonic acidifyings of water-bath 1 hour are transferred to sample solution in 125mL separating funnel after sample is cooling, add 20mL water to mix, 60mL normal hexane divides 3 extractions, and hexane extract is crossed anhydrous sodium sulfate dehydration, and 40 DEG C of Rotary Evaporators are concentrated into and are less than 2mL, shift solution to 10mL glass centrifuge tube, nitrogen dries up.
Add 1mL methyl alcohol dissolved residue, add the 100uL concentrated sulphuric acid to mix, 30 DEG C of heating water baths 20 minutes, add 2mL water, 1mL normal hexane, vortex mixes 1 minute, stratification, get normal hexane layer and do GC/MS analysis, measure the amount of methyl stearate, calculated the content of calcium stearate by the amount of methyl stearate.
2. set instrument parameter:
1) gas chromatograph condition
Gas chromatograph: Agilent 6890
Chromatographic column: HP-5MS capillary column 0.25mm × 30m × 0.25 μ m
Injector temperature: 280 DEG C
Flow rate of carrier gas: 1.0mL/min, constant current
Sample introduction pattern: Splitless injecting samples
Sampling volume: 1 μ L
Temperature programme: 100 DEG C of initial temperature, be warmed up to 300 DEG C by 30 DEG C of per minutes, keep 5 minutes.
2) mass spectrum condition
Solvent delay: 3min
Acquisition mode: SIM pattern
Ion source temperature: 230 DEG C
Quadrupole rod temperature: 150 DEG C
Scan ion m/z 74, m/z 87, m/z 298
3. quantitative and qualitative analysis
1) qualitative
Retention time through sample peak and standard items peak is compared, and the comparison of comparing of sample peak mass spectrogram and standard substance mass spectrogram determines in sample, whether to detect determinand.
2) quantitative
Adopt typical curve external standard method quantitative
4. calculate
Be 1 to carry out the calculating of calcium stearate content according to methyl stearate and calcium stearate reduction coefficient.
Embodiment 2: the mensuration of calcium stearate in injection microbiotic cefminox sodium
1. the preparation of sample:
Take even medicinal powder 4.0g, add 40ml water ultrasonic dissolution sample, pipette 2mL sample solution in 40mL vial, add 400 hydrochloric acid, mix, 60 DEG C of ultrasonic acidifyings of water-bath 1 hour are transferred to sample solution in 125mL separating funnel after sample is cooling, add 20mL water to mix, 60mL normal hexane divides 3 extractions, and hexane extract is crossed anhydrous sodium sulfate dehydration, and 40 DEG C of Rotary Evaporators are concentrated into and are less than 2mL, shift solution to 10mL glass centrifuge tube, nitrogen dries up.
Add 1mL methyl alcohol dissolved residue, add the 100uL concentrated sulphuric acid to mix, 30 DEG C of heating water baths 20 minutes, add 2mL water, 1mL normal hexane, vortex mixes 1 minute, stratification, get normal hexane layer and do GC/MS analysis, measure the amount of methyl stearate, calculated the content of calcium stearate by the amount of methyl stearate.
2. set instrument parameter:
1) gas chromatograph condition
Gas chromatograph: Agilent 6890
Chromatographic column: HP-5MS capillary column 0.25mm × 30m × 0.25 μ m
Injector temperature: 280 DEG C
Flow rate of carrier gas: 1.0mL/min, constant current
Sample introduction pattern: Splitless injecting samples
Sampling volume: 1 μ L
Temperature programme: 100 DEG C of initial temperature, be warmed up to 300 DEG C by 30 DEG C of per minutes, keep 5 minutes.
2) mass spectrum condition
Solvent delay: 3min
Acquisition mode: SIM pattern
Ion source temperature: 230 DEG C
Quadrupole rod temperature: 150 DEG C
Scan ion m/z 74, m/z 87, m/z 298
3. quantitative and qualitative analysis
1) qualitative
Retention time through sample peak and standard items peak is compared, and the comparison of comparing of sample peak mass spectrogram and standard substance mass spectrogram determines in sample, whether to detect determinand.
2) quantitative
Adopt typical curve external standard method quantitative
4. calculate
Be 1 to carry out the calculating of calcium stearate content according to methyl stearate and calcium stearate reduction coefficient.
As shown in Figures 1 and 2, be respectively gas chromatography, the mass spectrogram of methyl stearate, wherein, in Fig. 1, the peak of 5.5 minutes is the peak of methyl palmitate in sample liquid.
Embodiment 3: the mensuration of calcium stearate in injection microbiotic cefoxitin sodium
1. the preparation of sample:
Take even medicinal powder 4.0g, add 40ml water ultrasonic dissolution sample, pipette 2mL sample solution in 40mL vial, add 400 hydrochloric acid, mix, 60 DEG C of ultrasonic acidifyings of water-bath 1 hour are transferred to sample solution in 125mL separating funnel after sample is cooling, add 20mL water to mix, 60mL normal hexane divides 3 extractions, and hexane extract is crossed anhydrous sodium sulfate dehydration, and 40 DEG C of Rotary Evaporators are concentrated into and are less than 2mL, shift solution to 10mL glass centrifuge tube, nitrogen dries up.
Add 1mL methyl alcohol dissolved residue, add the 100uL concentrated sulphuric acid to mix, 30 DEG C of heating water baths 20 minutes, add 2mL water, 1mL normal hexane, vortex mixes 1 minute, stratification, get normal hexane layer and do GC/MS analysis, measure the amount of methyl stearate, calculated the content of calcium stearate by the amount of methyl stearate.
2. set instrument parameter:
1) gas chromatograph condition
Gas chromatograph: Agilent 6890
Chromatographic column: HP-5MS capillary column 0.25mm × 30m × 0.25 μ m
Injector temperature: 280 DEG C
Flow rate of carrier gas: 1.0mL/min, constant current
Sample introduction pattern: Splitless injecting samples
Sampling volume: 1 μ L
Temperature programme: 100 DEG C of initial temperature, be warmed up to 300 DEG C by 30 DEG C of per minutes, keep 5 minutes.
2) mass spectrum condition
Solvent delay: 3min
Acquisition mode: SIM pattern
Ion source temperature: 230 DEG C
Quadrupole rod temperature: 150 DEG C
Scan ion m/z 74, m/z 87, m/z 298
3. quantitative and qualitative analysis
1) qualitative
Retention time through sample peak and standard items peak is compared, and the comparison of comparing of sample peak mass spectrogram and standard substance mass spectrogram determines in sample, whether to detect determinand.
2) quantitative
Adopt typical curve external standard method quantitative
4. calculate
Be 1 to carry out the calculating of calcium stearate content according to methyl stearate and calcium stearate reduction coefficient.
Claims (3)
1. a method of measuring calcium stearate in medicine, is characterized in that, comprises the following steps:
1) sample pretreatment: extracting sample solution, add hcl acidifying, extract through normal hexane, obtain hexane extract, concentrated hexane extract rotary evaporation and nitrogen are blown to dry;
2) esterification: add methyl alcohol to dissolve, then add sulfuric acid to mix, with normal hexane extraction esterification product, vortex mixes, and stratification is got normal hexane layer;
3) adopt gas chromatograph-mass spectrometer determination step 2) amount of methyl stearate in the normal hexane layer of gained, the condition determination of gas chromatograph-mass spectrometer is: gas chromatographic column adopts HP-5MS capillary column, specification is 30 meters of column lengths, 0.25 millimeter of column internal diameter, 0.25 micron of thickness; Gas chromatographic sample introduction mouth Temperature Setting is 280 DEG C, and temperature programme is 100 DEG C of initial temperature, is warmed up to 300 DEG C by 30 DEG C of per minutes, retains 5 minutes; Ion scan pattern is selected in mass spectrum collection, and scan ion is m/z 74, m/z 87, m/z 298;
4) last, according to step 3) amount of the methyl stearate of gained, the content of calcium stearate in calculation sample solution, wherein, the reduction coefficient of calcium stearate and methyl stearate
2. the method for claim 1, is characterized in that: step 1) in, sample is solution-type medicine or parenteral solution, draw sample solution, add hydrochloric acid, mix, 60 DEG C of ultrasonic acidifyings of water-bath 1 hour, after cooling sample solution is transferred in separating funnel, adds water and mixes, divide 3 extractions through normal hexane, hexane extract is crossed to anhydrous sodium sulfate dehydration, 40 DEG C of Rotary Evaporators are concentrated into and are less than 2mL, shift solution to glass centrifuge tube, and nitrogen dries up.
3. the method for claim 1, it is characterized in that: step 1) in, sample is solid medicine, take even medicinal powder, add water ultrasonic dissolution sample, obtain sample solution, pipette sample solution in vial, add hydrochloric acid, mix, 60 DEG C of ultrasonic acidifyings of water-bath 1 hour, are transferred to sample solution in separating funnel after cooling, add water and mix, divide 3 extractions through normal hexane, hexane extract is crossed to anhydrous sodium sulfate dehydration, 40 DEG C of Rotary Evaporators are concentrated into and are less than 2mL, shift solution to glass centrifuge tube, nitrogen dries up.
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| KR20170011781A (en) * | 2015-07-24 | 2017-02-02 | 주식회사 엘지화학 | A method for quantitive analysis of metal stearate in polymer and composition therefor |
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| CN108195987B (en) * | 2018-01-15 | 2021-01-01 | 黄河三角洲京博化工研究院有限公司 | Method for analyzing stearic acid content in stearate |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102539609A (en) * | 2011-12-31 | 2012-07-04 | 青岛啤酒股份有限公司 | Detection method for measuring free fatty acid in beer through methyl esterification in bottle-headspace SPME (solid-phase micro-extraction)-gas chromatography and mass spectrum |
| CN102841171A (en) * | 2012-09-03 | 2012-12-26 | 湖南农业大学 | Detection method for tea seed oil adulteration based on ratio of main fatty acids |
-
2013
- 2013-05-31 CN CN201310211968.4A patent/CN103293242B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102539609A (en) * | 2011-12-31 | 2012-07-04 | 青岛啤酒股份有限公司 | Detection method for measuring free fatty acid in beer through methyl esterification in bottle-headspace SPME (solid-phase micro-extraction)-gas chromatography and mass spectrum |
| CN102841171A (en) * | 2012-09-03 | 2012-12-26 | 湖南农业大学 | Detection method for tea seed oil adulteration based on ratio of main fatty acids |
Non-Patent Citations (12)
| Title |
|---|
| Ali RANJI et al..Determination of Calcium Stearate in Polyolefin Samples by Gas Chromatographic Technique after Performing dispersive Liquid–Liquid Microextraction.《ANALYTICAL SCIENCES》.2008,第24卷 * |
| Determination of Calcium Stearate in Polyolefin Samples by Gas Chromatographic Technique after Performing dispersive Liquid–Liquid Microextraction;Ali RANJI et al.;《ANALYTICAL SCIENCES》;20080531;第24卷;第623-626页 * |
| Gas chromatographic determination of calcium stearate in polyethylene food packaging sheets;SHIGERU TAN et al.;《Journal of Chromatography》;19881231;第447卷;第198-201页 * |
| SHIGERU TAN et al..Gas chromatographic determination of calcium stearate in polyethylene food packaging sheets.《Journal of Chromatography》.1988,第447卷 * |
| 姚崇林 等.食品中硬脂酸镁气相色谱法测定.《中国公共卫生》.2006,第22卷(第2期), * |
| 徐文东 等.药用辅料油酸钠中反式脂肪酸的GC-MS分析.《北方药学》.2012,第9卷(第8期), * |
| 李英 等.气相色谱-质谱法测定混合脂肪酸钠盐中脂肪酸的组成.《质谱学报》.2003,第24卷(第2期), * |
| 气相色谱-质谱法测定混合脂肪酸钠盐中脂肪酸的组成;李英 等;《质谱学报》;20030531;第24卷(第2期);第351-355页 * |
| 气相色谱-质谱联用分析八角茴香中脂肪酸;赵丽娟;《食品科学》;20121231;第33卷(第12期);第250-253页 * |
| 药用辅料油酸钠中反式脂肪酸的GC-MS分析;徐文东 等;《北方药学》;20121231;第9卷(第8期);第7-8页 * |
| 赵丽娟.气相色谱-质谱联用分析八角茴香中脂肪酸.《食品科学》.2012,第33卷(第12期), * |
| 食品中硬脂酸镁气相色谱法测定;姚崇林 等;《中国公共卫生》;20060228;第22卷(第2期);第244页 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20170011781A (en) * | 2015-07-24 | 2017-02-02 | 주식회사 엘지화학 | A method for quantitive analysis of metal stearate in polymer and composition therefor |
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