CN103776915A - Method for measuring residual quantity of trifluoroacetic acid in epirubicin hydrochloride - Google Patents
Method for measuring residual quantity of trifluoroacetic acid in epirubicin hydrochloride Download PDFInfo
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- CN103776915A CN103776915A CN201310569603.9A CN201310569603A CN103776915A CN 103776915 A CN103776915 A CN 103776915A CN 201310569603 A CN201310569603 A CN 201310569603A CN 103776915 A CN103776915 A CN 103776915A
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Abstract
The invention discloses a method for measuring residual quantity of trifluoroacetic acid in epirubicin hydrochloride. The method adopts a gas chromatographic method, a capillary column is selected and used, an electron capture detector (ECD) is adopted, sulphuric acid-methanol, methyl sulfate and methyl iodide are used as methyl esterification reagents, and the trifluoroacetic acid is subjected to methyl esterification to generate methyl trifluoroacetate suitable for headspace sampling. Compared with the prior art, the method provided by the invention can be applied to measurement of content of the trifluoroacetic acid in epirubicin hydrochloride.
Description
Technical field
The present invention relates to Pharmaceutical Analysis technology, more specifically, relate to a kind of assay method of crossing fluoroacetic acid residual quantity in Farmorubine Hydrochloride.
Background technology
Crossing fluoroacetic 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, amino acid protection, organic synthesis, the fields such as material processed are widely used.Intermediate as fluorine-containing medicines, agricultural chemicals and dyestuff is excellent active because trifluoromethyl group shows in fluorine-containing medicines, agricultural chemicals, dyestuff, crosses fluoroacetic acid as the primary raw material of introducing trifluoromethyl group.
Epi-ADM belongs to antibiotics anticarcinogen, and its mechanism of action comprises the synthetic mitosis of being combined with DNA and suppressing nucleic acid.In addition Epi-ADM also can suppress topoisomerase, and shows the active anticancer of wide spectrum, and its cardiac toxic is lower.
Owing to can have the residual of fluoroacetic acid in Farmorubine Hydrochloride preparation process, stipulate according to " Chinese Pharmacopoeia ", cross fluoroacetic acid and divide the 4th kind solvent that there is no enough toxicological informations into, should be according to the feature of production technology, formulate corresponding limit, make it meet product specification, GMP (GMP) or other basic quality requirementss.
The existing method that detected fluoroacetic acid:
1), after medicine being carried out to oxygen bottle burning and destroying, measure fluorine with Colorimetry, then be converted into the method for fluoroacetic acid content;
2) chromatography of ions, principle is to utilize fluoroacetic acid to be different from the conductivity of other negative ion, uses conductance cell detecting device to carry out quantitative and qualitative analysis to crossing fluoroacetic 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 compared with method 2.
Summary of the invention
The object of invention is to provide a kind of method of crossing fluoroacetic acid content in Farmorubine Hydrochloride of measuring with gc analysis, can be used for the quality control of product in Farmorubine Hydrochloride.
The invention provides a kind of method with crossing fluoroacetic acid content in gas chromatography determination Farmorubine Hydrochloride, 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 crossing fluoroacetic acid content in gas chromatography determination Farmorubine Hydrochloride, 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 crossing fluoroacetic acid content in gas chromatography determination Farmorubine Hydrochloride, 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 crossing fluoroacetic acid content in gas chromatography determination Farmorubine Hydrochloride, the temperature of wherein said esterification is 60 ~ 85 ℃.
The invention provides a kind of method with crossing fluoroacetic acid content in gas chromatography determination Farmorubine Hydrochloride, wherein the temperature of headspace sampling sample introduction head space bottle is 45 ~ 55 ℃.
The invention provides a kind of method with crossing fluoroacetic acid content in gas chromatography determination Farmorubine Hydrochloride, comprise the steps:
1) get test sample in right amount to 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 for 60 minutes, preferably 80 ℃ of water-baths.
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 DB-624 capillary column.
4) when 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 sample crosses the mensuration of fluoroacetic acid content.
Here the volume ratio of sulfuric acid-methyl alcohol is 1 ~ 12:99 ~ 88, preferably 10:90, and the volume ratio of dimethyl suflfate-methyl alcohol is 0.5 ~ 6:99.5 ~ 96, preferably 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 crossing fluoroacetic acid content in gas chromatography determination Farmorubine Hydrochloride, comprise the steps:
1) get test sample in right amount to 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 for 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 DB-624 capillary column.
4), when headspace sampling, the temperature of head space bottle is 55 ℃.
5) extract head space bottle upper gas 0.1ml, inject gas chromatograph completes sample crosses the mensuration of fluoroacetic 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.
After jasmine discloses medicine is carried out to the burning of oxygen bottle and destroys, measure fluorine with Colorimetry, then be converted into the method for fluoroacetic acid content.(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 fluoroacetic acid become inorganic fluorion, measure fluorine with Colorimetry, be converted into again the amount of fluoroacetic acid, but the method use there is limitation.Should be the method will carry out oxygen bottle burning destruction to sample, is only applicable to not contain in drug molecular structure the organic compound of fluorine element, if contain fluorine element in test compound molecule, cannot detect it.Detection method provided by the invention, has improved the specificity of measuring, and has avoided the interference to test findings of the fluorine element that contains in molecular structure.
Accompanying drawing explanation: the gas chromatogram that Fig. 1 is sulfuric acid-methyl alcohol;
Fig. 2 was that fluoroacetic acid is through derivative gas chromatogram;
Fig. 3 was the gas chromatogram of methylfluoracetate;
Fig. 4 is the gas chromatogram of sample 1;
Fig. 5 is the gas chromatogram of 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 departing 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 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 the above-mentioned condition of test sample photograph and carry out gas phase analysis, record chromatogram, in mistake, going out on peak position of methylfluoracetate do not have chromatographic peak, the results are shown in Figure 1.
Embodiment 2
Instrument and condition
Clarus500GC type gas chromatograph is joined 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 the 10% sulfuric acid-methanol solution 2ml top set empty bottle that contained fluoroacetic acid 4.0ug/ml 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 chromatographic peak that retention time is 6.18min was that fluoroacetic acid process is derivative, and the chromatographic peak of crossing methylfluoracetate of generation, the results are shown in Figure 2.
Embodiment 3
Instrument and condition
Clarus500GC type gas chromatograph is joined 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 contained methylfluoracetate 1ug/ml, makes it to dissolve in top set empty bottle, 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 the chromatographic peak that retention time is 6.21min was methylfluoracetate, the results are shown in Figure 3.
Embodiment 4
Instrument and condition
Clarus500GC type gas chromatograph is joined 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 20mg in test sample Farmorubine Hydrochloride, 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, crossing the methylfluoracetate of crossing that did not detect the derivative rear generation of fluoroacetic acid on peak position that of methylfluoracetate, the results are shown in Figure 4.
Embodiment 5
Instrument and condition
Clarus500GC type gas chromatograph is joined 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 19.8mg in test sample Farmorubine Hydrochloride, 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, crossing the methylfluoracetate of crossing that did not detect the derivative rear generation of fluoroacetic acid on peak position that of methylfluoracetate, the results are shown in Figure 5.
Embodiment 6
Instrument and condition
Clarus500GC type gas chromatograph is joined 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 20.6mg in test sample Farmorubine Hydrochloride, 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 did not detect the methylfluoracetate of crossing of the derivative rear generation of fluoroacetic acid.
Embodiment 7
Instrument and condition
Clarus500GC type gas chromatograph is joined 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 19.7mg in test sample Farmorubine Hydrochloride, 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 did not detect the methylfluoracetate of crossing of the derivative rear generation of fluoroacetic acid.
Claims (9)
1. a method of crossing fluoroacetic acid content in gas chromatography determination Farmorubine Hydrochloride, is characterized in that the capillary column with DB-624, take ECD as detecting device, sulfuric acid-methyl alcohol, 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 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. a method of crossing fluoroacetic acid content in gas chromatography determination Farmorubine Hydrochloride, comprises the steps:
1) get test sample in right amount to 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 for 60 minutes, preferably 80 ℃ of water-baths;
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 DB-624 capillary column;
4) when 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 sample crosses the mensuration of fluoroacetic acid content.
9. a method of crossing fluoroacetic acid content in gas chromatography determination Farmorubine Hydrochloride, comprises the steps:
1) get test sample in right amount to 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 for 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 DB-624 capillary column;
4), when headspace sampling, the temperature of head space bottle is 55 ℃;
5) extract head space bottle upper gas 0.1ml inject gas chromatograph and complete sample and cross the mensuration of fluoroacetic acid content.
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|---|---|---|---|
| CN201310569603.9A CN103776915A (en) | 2013-11-13 | 2013-11-13 | Method for measuring residual quantity of trifluoroacetic acid in epirubicin hydrochloride |
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| CN201310569603.9A CN103776915A (en) | 2013-11-13 | 2013-11-13 | Method for measuring residual quantity of trifluoroacetic acid in epirubicin hydrochloride |
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| CN201310569603.9A Pending CN103776915A (en) | 2013-11-13 | 2013-11-13 | Method for measuring residual quantity of trifluoroacetic acid in epirubicin hydrochloride |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0611498A (en) * | 1992-06-26 | 1994-01-21 | Hitachi Ltd | Gas chromatographic method and gas chromatograph mass-spectrometric method |
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2013
- 2013-11-13 CN CN201310569603.9A patent/CN103776915A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0611498A (en) * | 1992-06-26 | 1994-01-21 | Hitachi Ltd | Gas chromatographic method and gas chromatograph mass-spectrometric method |
Non-Patent Citations (4)
| Title |
|---|
| CHAD E.WUJCIK ET AL.: "Extraction and analysis of trifluoroacetic acid in environmental waters", 《ANAL.CHEM.》 * |
| WULF AMELUNG ET AL.: "DETERMINATION OF NEUTRAL AND ACIDIC SUGARS IN SOIL BY CAPILLARY GAS-LIQUID CHROMATOGRAPHY AFTER TRIFLUOROACETIC ACID HYDROLYSIS", 《SOIL BIOL. BIOCHEM.》 * |
| 冯建林 等: "气相色谱和气相色谱-质谱联用法测定药物扶素康中的三氟醋酸", 《分析测试学报》 * |
| 张莉 等: "有机药物中残留三氟醋酸测定方法的研究", 《华西药学杂志》 * |
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Application publication date: 20140507 |