CN103439427A - Method for measuring residual amount of trifluoroacetic acid in celecoxib - Google Patents
Method for measuring residual amount of trifluoroacetic acid in celecoxib Download PDFInfo
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- CN103439427A CN103439427A CN201310384149XA CN201310384149A CN103439427A CN 103439427 A CN103439427 A CN 103439427A CN 201310384149X A CN201310384149X A CN 201310384149XA CN 201310384149 A CN201310384149 A CN 201310384149A CN 103439427 A CN103439427 A CN 103439427A
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Abstract
The invention discloses a method for measuring the residual amount of trifluoroacetic acid in celecoxib. The method comprises the following steps of: by using a gas chromatographic method, selecting a capillary column, using an ECD (electron capture detector) as a detector, using sulphuric acid-methanol, dimethyl sulphate and iodomethane as methyl esterification reagents, and generating methyl trifluoroacetate suitable for headspace sampling from trifluoroacetic acid via esterification. Compared with the prior art, the method disclosed by the invention can be used for measuring the content of trifluoroacetic acid in celecoxib.
Description
Technical field
The present invention relates to the Pharmaceutical Analysis technology, more specifically, relate to the method for trifluoroacetic acid content in a kind of gas chromatography determination Sai-Mi-Xi-Bu.
Background technology
Trifluoroacetic acid is a kind of extremely strong acid organic acid, has a lot of inorganicss and organic ability simultaneously, makes it to have excellent reactivity worth, thus at medicine, agricultural chemicals, fuel, the amino acid protection, organic synthesis, the fields such as material processed are widely used.Intermediate as fluorine-containing medicines, agricultural chemicals and dyestuff shows excellent activity in fluorine-containing medicines, agricultural chemicals, dyestuff due to trifluoromethyl group, trifluoroacetic acid is as the primary raw material of introducing trifluoromethyl group.
Sai-Mi-Xi-Bu is a kind of NSAID of a new generation, has unique mechanism of action and suppresses specifically COX-2.Reach anti-inflammatory, analgesia and antipyretic effect.Owing in the Sai-Mi-Xi-Bu preparation process, can having the residual of trifluoroacetic acid.
According to " Chinese pharmacopoeia regulation, trifluoroacetic acid divides into, there is no the 4th kind solvent of enough toxicological informations, should be according to the characteristics of production technology, formulate corresponding limit, make it meet product specification, GMP (GMP) or other basic quality requirementss.
The existing method that detects trifluoroacetic acid:
1) after medicine being carried out to oxygen bottle burning destruction, measure fluorine with Colorimetry, then be converted into the method for trifluoroacetic acid content.
2) chromatography of ions, principle is to utilize trifluoroacetic acid to be different from the conductivity of other negative ion, uses the conductance cell detecting device to carry out quantitative and qualitative analysis to trifluoroacetic acid.
Compared with the conventional method, this method can be avoided using method 1, causes the interference of fluorine element to testing result in molecular structure, can also reach the detection sensitivity higher than method 2.
Summary of the invention
The purpose of invention is to provide a kind of method of measuring trifluoroacetic acid content in Sai-Mi-Xi-Bu with gc analysis, can be used for the quality control of Sai-Mi-Xi-Bu product.
The invention provides a kind of method with trifluoroacetic acid content in the gas chromatography determination Sai-Mi-Xi-Bu, adopt capillary column, take ECD as detecting device, sulfuric acid-methyl alcohol or dimethyl suflfate-methyl alcohol, iodomethane-methyl alcohol are solvent.
The invention provides a kind of method with trifluoroacetic acid content in the gas chromatography determination Sai-Mi-Xi-Bu, the concentration that wherein volume ratio of solvent sulfuric acid-methyl alcohol is is 1 ~ 12:99 ~ 88, the concentration that the volume ratio of dimethyl suflfate-methyl alcohol is is 0.5 ~ 6:99.5 ~ 94, and the concentration that the volume ratio of iodomethane-methyl alcohol is is 0.5 ~ 6:99.5 ~ 94.
The invention provides a kind of method with trifluoroacetic acid content in the gas chromatography determination Sai-Mi-Xi-Bu, the concentration that wherein volume ratio of solvent sulfuric acid-methyl alcohol is is 10:90, the concentration that the volume ratio of dimethyl suflfate-methyl alcohol is is 5:95, and the concentration that the volume ratio of iodomethane-methyl alcohol is is 5:95.
The invention provides a kind of method with trifluoroacetic acid content in the gas chromatography determination Sai-Mi-Xi-Bu, the temperature of wherein said esterification is 60 ~ 85 ℃.
The invention provides a kind of method with trifluoroacetic acid content in the gas chromatography determination Sai-Mi-Xi-Bu, wherein the temperature of headspace sampling sample introduction head space bottle is 45 ~ 55 ℃.
The invention provides a kind of method with trifluoroacetic acid content in the gas chromatography determination Sai-Mi-Xi-Bu, comprise the steps:
1) get test sample in right amount to the headspace sampling bottle, add sulfuric acid-methyl alcohol or dimethyl suflfate-methyl alcohol, iodomethane-dissolve with methanol solution is made the sample solution of every 1ml containing test sample 10mg.
2) the head space bottle after gland is put to 60 ~ 85 ℃ of heating water baths and derived in 60 minutes, preferably water-bath is 80 ℃.
3) column temperature is set and is initially 60 ℃, keep 10 minutes, then rise to 235 ℃ with the speed of 40 ℃ of per minute intensifications, keep 5 minutes; Injector temperature is 140 ℃; Detecting device is ECD; Detector temperature is 250 ~ 350 ℃, and optimum temperature is 350 ℃; Chromatographic column is the DB-624 capillary column.
4) during headspace sampling, the temperature of head space bottle is 45 ~ 55 ℃, and optimum temperature is 55 ℃.
5) extract head space bottle upper gas 0.1 ~ 1.0ml, be preferably 0.1ml, inject gas chromatograph completes the mensuration of sample trifluoroacetic acid content.
Here the volume ratio of sulfuric acid-methyl alcohol is 1 ~ 12:99 ~ 88, preferred 10:90, and the volume ratio of dimethyl suflfate-methyl alcohol is 0.5 ~ 6:99.5 ~ 96, preferred 5:95, the volume ratio of iodomethane-methyl alcohol is 0.5 ~ 6:99.5 ~ 96, preferably 5:95.
The invention provides a kind of method with trifluoroacetic acid content in the gas chromatography determination Sai-Mi-Xi-Bu, comprise the steps:
1) get test sample in right amount to the headspace sampling bottle, add sulfuric acid-dissolve with methanol solution and make the sample solution of every 1ml containing test sample 10mg.
2) the head space bottle after gland is put to 80 ℃ of heating water baths derives in 60 minutes.
3) column temperature is set and is initially 60 ℃, keep 10 minutes, then rise to 235 ℃ with the speed of 40 ℃ of per minute intensifications, keep 5 minutes; Injector temperature is 140 ℃; Detecting device is ECD; Detector temperature is 350 ℃, and chromatographic column is the DB-624 capillary column.
4), during headspace sampling, the temperature of head space bottle is 55 ℃.
5) extract head space bottle upper gas 0.1ml, inject gas chromatograph completes the mensuration of sample trifluoroacetic acid content.
Here the volume ratio of sulfuric acid methyl alcohol is 10:90, and the volume ratio of dimethyl suflfate-methyl alcohol is 5:95, and the volume ratio of iodomethane-methyl alcohol is 5:95.
Jasmine is measured fluorine with Colorimetry, then is converted into the method for trifluoroacetic acid content after disclosing medicine being carried out to the burning of oxygen bottle and destroys.(West China Journal of Pharmaceutical Sciences 2001,16(6): 427 ~ 428) the method is destroyed sample with the burning of oxygen bottle, makes the fluorine in trifluoroacetic acid become inorganic fluorion, with Colorimetry, measures fluorine, be converted into again the amount of trifluoroacetic acid, yet the method use there is limitation.Destroy because the method will be carried out the burning of oxygen bottle to sample, be only applicable to not contain in drug molecular structure the organic compound of fluorine element, if contain fluorine element in the test compound molecule can't be detected it.Detection method provided by the invention, improved the specificity of measuring, and avoided the interference to test findings of the fluorine element that contains in the molecular structure.
The accompanying drawing explanation:
The gas chromatogram that Fig. 1 is sulfuric acid-methyl alcohol;
Fig. 2 is that trifluoroacetic acid is through derivative gas chromatogram;
The gas chromatogram that Fig. 3 is trifluoro-acetate;
The gas chromatogram that Fig. 4 is sample 1;
The gas chromatogram that Fig. 5 is sample 2.
Form is described in further detail content of the present invention more by the following examples, but should not be interpreted as in the above-mentioned subject area of the present invention at this point and only limit to following examples.Do not breaking away under the above-mentioned technology prerequisite of the present invention, the corresponding replacement of making according to ordinary skill knowledge and customary means or the modification of change, include within the scope of the invention
.
Embodiment 1
Instrument and condition
Clarus500GC type gas chromatograph is joined the ECD detecting device, Turbomatrix40 type head-space sampler, DB-624 quartz capillary column chromatographic column.
Chromatographic condition: column temperature is initially 60 ℃, keeps 10 minutes, then rises to 235 ℃ with the speed of 40 ℃ of per minute intensifications, keeps 5 minutes; Sample introduction temperature: 140 ℃; Detecting device: ECD; Detector temperature: 350 ℃; Carrier gas: N
2.
Head space condition: furnace temp: 55 ℃, sample size 0.1ml.
Test procedure
Precision adds in 10% sulfuric acid-methanol solution 2ml top set empty bottle, and sealing, as need testing solution.
Head space bottle after gland is put to 80 ℃ of heating water baths and within 60 minutes, derive, place room temperature.
Get test sample and carry out gas phase analysis according to above-mentioned condition, record chromatogram, the results are shown in Figure 1(and go out on peak position not have chromatographic peak at trifluoro-acetate).
Embodiment 2
Instrument and condition
Clarus500GC type gas chromatograph is joined the ECD detecting device, Turbomatrix40 type head-space sampler, DB-624 quartz capillary column chromatographic column.
Chromatographic condition: column temperature is initially 60 ℃, keeps 10 minutes, then rises to 235 ℃ with the speed of 40 ℃ of per minute intensifications, keeps 5 minutes; Sample introduction temperature: 140 ℃; Detecting device: ECD; Detector temperature: 350 ℃; Carrier gas: N
2.
Head space condition: furnace temp: 55 ℃, sample size 0.1ml.
Test procedure
Precision adds in 10% sulfuric acid that contains trifluoroacetic acid 4.0ug/ml-methanol solution 2ml top set empty bottle to be made it to dissolve, and sealing, as need testing solution.
Head space bottle after gland is put to 80 ℃ of heating water baths and within 60 minutes, derive, place room temperature.
Get test sample and carry out gas phase analysis according to above-mentioned condition, record chromatogram, the results are shown in Figure the chromatographic peak that in 2(Fig. 2, retention time is 6.18min is that the trifluoroacetic acid process is derivative, the chromatographic peak of the trifluoro-acetate of generation).
Embodiment 3
Instrument and condition
Clarus500GC type gas chromatograph is joined the ECD detecting device, Turbomatrix40 type head-space sampler, DB-624 quartz capillary column chromatographic column.
Chromatographic condition: column temperature is initially 60 ℃, keeps 10 minutes, then rises to 235 ℃ with the speed of 40 ℃ of per minute intensifications, keeps 5 minutes; Sample introduction temperature: 140 ℃; Detecting device: ECD; Detector temperature: 350 ℃; Carrier gas: N
2.
Head space condition: furnace temp: 55 ℃, sample size 0.1ml.
Test procedure
Precision adds the methanol solution 2ml that contains trifluoro-acetate 1ug/ml, in the top set empty bottle, makes it to dissolve, and sealing, as need testing solution.
Get test sample and carry out gas phase analysis according to above-mentioned condition, record chromatogram, the chromatographic peak that to the results are shown in Figure chromatographic peak that in 3(Fig. 3, retention time is 6.21min be trifluoro-acetate).
Embodiment 4
Instrument and condition
Clarus500GC type gas chromatograph is joined the ECD detecting device, Turbomatrix40 type head-space sampler, DB-624 quartz capillary column chromatographic column.
Chromatographic condition: column temperature is initially 60 ℃, keeps 10 minutes, then rises to 235 ℃ with the speed of 40 ℃ of per minute intensifications, keeps 5 minutes; Sample introduction temperature: 140 ℃; Detecting device: ECD; Detector temperature: 350 ℃; Carrier gas: N
2.
Head space condition: furnace temp: 55 ℃, sample size 0.1ml.
Test procedure
Get test sample Sai-Mi-Xi-Bu 20mg, accurately weighed, precision adds in 10% sulfuric acid-methanol solution 2ml top set empty bottle to be made it to dissolve, and sealing, as need testing solution.
Head space bottle after gland is put to 80 ℃ of heating water baths and within 60 minutes, derive, place room temperature.
Get test sample and carry out gas phase analysis according to above-mentioned condition, record chromatogram, the results are shown in Figure the trifluoro-acetate that go out peak position on do not detect trifluoroacetic acid derivative rear generation of 4(at trifluoro-acetate).
Embodiment 5
Instrument and condition
Clarus500GC type gas chromatograph is joined the ECD detecting device, Turbomatrix40 type head-space sampler, DB-624 quartz capillary column chromatographic column.
Chromatographic condition: column temperature is initially 60 ℃, keeps 10 minutes, then rises to 235 ℃ with the speed of 40 ℃ of per minute intensifications, keeps 5 minutes; Sample introduction temperature: 140 ℃; Detecting device: ECD; Detector temperature: 350 ℃; Carrier gas: N
2.
Head space condition: furnace temp: 55 ℃, sample size 0.1ml.
Test procedure
Get test sample Sai-Mi-Xi-Bu 19.8mg, accurately weighed, precision adds in 10% sulfuric acid-methanol solution 2ml top set empty bottle to be made it to dissolve, and sealing, as need testing solution.
Head space bottle after gland is put to 80 ℃ of heating water baths and within 60 minutes, derive, place room temperature.
Get test sample and carry out gas phase analysis according to above-mentioned condition, record chromatogram, the results are shown in Figure the trifluoro-acetate that go out peak position on do not detect trifluoroacetic acid derivative rear generation of 5(at trifluoro-acetate).
Embodiment 6
Instrument and condition
Clarus500GC type gas chromatograph is joined the ECD detecting device, Turbomatrix40 type head-space sampler, DB-624 quartz capillary column chromatographic column.
Chromatographic condition: column temperature is initially 60 ℃, keeps 10 minutes, then rises to 235 ℃ with the speed of 40 ℃ of per minute intensifications, keeps 5 minutes; Sample introduction temperature: 140 ℃; Detecting device: ECD; Detector temperature: 350 ℃; Carrier gas: N
2.
Head space condition: furnace temp: 55 ℃, sample size 0.1ml.
Test procedure
Get test sample Sai-Mi-Xi-Bu 20.7mg, accurately weighed, precision adds in 5% dimethyl suflfate-methanol solution 2ml top set empty bottle to be made it to dissolve, and sealing, as need testing solution.
Head space bottle after gland is put to 80 ℃ of heating water baths and within 60 minutes, derive, place room temperature.
Get test sample and carry out gas phase analysis according to above-mentioned condition, record chromatogram, result does not detect the derivative rear trifluoro-acetate generated of trifluoroacetic acid.
Embodiment 7
Instrument and condition
Clarus500GC type gas chromatograph is joined the ECD detecting device, Turbomatrix40 type head-space sampler, DB-624 quartz capillary column chromatographic column.
Chromatographic condition: column temperature is initially 60 ℃, keeps 10 minutes, then rises to 235 ℃ with the speed of 40 ℃ of per minute intensifications, keeps 5 minutes; Sample introduction temperature: 140 ℃; Detecting device: ECD; Detector temperature: 350 ℃; Carrier gas: N
2.
Head space condition: furnace temp: 55 ℃, sample size 0.1ml.
Test procedure
Get test sample Sai-Mi-Xi-Bu 20.2mg, accurately weighed, precision adds in 5% iodomethane-methanol solution 2ml top set empty bottle to be made it to dissolve, and sealing, as need testing solution.
Head space bottle after gland is put to 80 ℃ of heating water baths and within 60 minutes, derive, place room temperature.
Get test sample and carry out gas phase analysis according to above-mentioned condition, record chromatogram, result does not detect the derivative rear trifluoro-acetate generated of trifluoroacetic acid.
Claims (9)
1. the method for trifluoroacetic acid content in a gas chromatography determination Sai-Mi-Xi-Bu, is characterized in that the capillary column with DB-624, take ECD as detecting device, sulfuric acid-methyl alcohol, and dimethyl suflfate, iodomethane is methyl esterification reagent, sample is through insulation esterification, headspace sampling.
2. method according to claim 1, wherein, in solvent sulfuric acid-methanol solution, the concentration that the volume ratio of sulfuric acid and methyl alcohol is is 1 ~ 12:99 ~ 88, dimethyl suflfate-methyl alcohol 0.5 ~ 6:99.5 ~ 94, iodomethane-methyl alcohol 0.5 ~ 6:99.5 ~ 94.
3. method according to claim 2, wherein, the ratio of sulfuric acid and methyl alcohol is 10:90, dimethyl suflfate-methyl alcohol 5:95, iodomethane-methyl alcohol 5:95.
4. method according to claim 1, sample is through the insulation esterification, and the temperature of esterification is 60 ~ 85 ℃.
5. method according to claim 4, wherein, the temperature of esterification is 80 ℃.
6. method according to claim 1, the sample headspace sample introduction after esterification, the temperature of sample introduction head space bottle is 45 ~ 55 ℃.
7. method according to claim 6, wherein, the temperature of the head space bottle of sample introduction is 50 ℃.
8. the method for trifluoroacetic acid content in a gas chromatography determination Sai-Mi-Xi-Bu, comprise the steps:
(1) get test sample in right amount to the headspace sampling bottle, add sulfuric acid-methyl alcohol or dimethyl suflfate-methyl alcohol, iodomethane-dissolve with methanol solution is made the sample solution of every 1ml containing test sample 10mg;
(2) the head space bottle after gland is put to 60 ~ 85 ℃ of heating water baths and derived in 60 minutes, preferably water-bath is 80 ℃;
(3) column temperature is set and is initially 60 ℃, keep 10 minutes, then rise to 235 ℃ with the speed of 40 ℃ of per minute intensifications, keep 5 minutes; Injector temperature is 140 ℃; Detecting device is ECD; Detector temperature is 250 ~ 350 ℃, and optimum temperature is 350 ℃; Chromatographic column is the DB-624 capillary column;
(4) during headspace sampling, the temperature of head space bottle is 45 ~ 55 ℃, and optimum temperature is 55 ℃;
(5) extract head space bottle upper gas 0.1 ~ 1.0ml, be preferably 0.1ml, inject gas chromatograph completes the mensuration of sample trifluoroacetic acid content.
9. the method for trifluoroacetic acid content in a gas chromatography determination Sai-Mi-Xi-Bu, comprise the steps:
(1) get test sample in right amount to the headspace sampling bottle, add sulfuric acid-methyl alcohol or dimethyl suflfate-methyl alcohol, iodomethane-dissolve with methanol solution is made the sample solution of every 1ml containing test sample 10mg;
(2) the head space bottle after gland is put to 80 ℃ of heating water baths derives in 60 minutes;
(3) column temperature is set and is initially 60 ℃, keep 10 minutes, then rise to 235 ℃ with the speed of 40 ℃ of per minute intensifications, keep 5 minutes; Injector temperature is 140 ℃; Detecting device is ECD; Detector temperature is 350 ℃; Chromatographic column is the DB-624 capillary column;
(4), during headspace sampling, the temperature of head space bottle is 55 ℃;
(5) extract the mensuration that head space bottle upper gas 0.1ml inject gas chromatograph completes sample trifluoroacetic acid content.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103776920A (en) * | 2013-11-13 | 2014-05-07 | 江苏正大清江制药有限公司 | Method for measuring trifluoroacetic acid residual quantity in ganirelix acetate |
-
2013
- 2013-08-30 CN CN201310384149XA patent/CN103439427A/en active Pending
Non-Patent Citations (5)
| Title |
|---|
| CHAD E.WUJCIK等: "Extraction and analysis of trifluoroacetic acid in environmental waters", 《ANAL.CHEM.》 * |
| EPA: "Determination of Haloacetic Acids and Dalapon in Drinking Water by Liquid-Liquid Microextraction, Derivatization, and Gas Chromatography with Electron capture Detection", 《EPA 815-B-03-002》 * |
| THOMAS M.CAHILL等: "Simplified Method for Trace Analysis of Trifluoroacetic Acid in Plant, Soil, and Water Samples Using Headspace Gas Chromatography", 《ANAL.CHEM.》 * |
| 张颖等: "环境水体中三氟乙酸的存在现状及分析方法的研究", 《中国环境监测》 * |
| 朱圣亮等: "柱前衍生化顶空气相色谱法同时检测非布司他原料药中3种微量有机酸", 《中国药房》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103776920A (en) * | 2013-11-13 | 2014-05-07 | 江苏正大清江制药有限公司 | Method for measuring trifluoroacetic acid residual quantity in ganirelix acetate |
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Application publication date: 20131211 |