CN113720956B - Method for detecting sulfate in medicine by gas chromatography-mass spectrometry - Google Patents
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Abstract
The application belongs to the technical field of medicine detection and analysis. The application provides a method for detecting sulfate in a medicament by gas chromatography-mass spectrometry. The method comprises the steps of dissolving a test sample by using a first organic solvent and an acid solution, adjusting the ionic strength by using a salt solution and a second organic solvent, carrying out liquid-liquid extraction, and detecting the content of sulfate compounds in the obtained test sample solution by using a gas chromatograph-mass spectrometer. The detection method is simple and convenient to operate, consumes less time, is verified by methodology, has good specificity, linearity, accuracy, sensitivity and stability, and meets the requirement of measuring the content of sulfate compounds in the medicine.
Description
Technical Field
The application belongs to the technical field of medicine detection and analysis, and particularly relates to a method for detecting sulfate in a medicine by gas chromatography-mass spectrometry.
Background
Sulfuric acid esters are a class of compounds in which the hydrogen atom of a hydroxyl group in sulfuric acid is replaced by a hydrocarbyl group. The most important industrially important alkyl sulfates are dimethyl sulfate and diethyl sulfate, which are also important raw materials in the preparation of pharmaceuticals. The sulfate has strong corrosivity, the residue of sulfate in the medicine is bound to cause serious harm to human health, and the limit of dimethyl sulfate and diethyl sulfate does not exceed 0.75ppm, so the residual concentration of sulfate compounds in the medicine needs to be strictly monitored.
Because the polarity of the sulfate compounds is large and the detection is easy to interfere, the detection method of sulfate in the medicine is mainly a derivatization liquid phase method, a liquid phase method and a gas phase method at present, although the detection stability of the derivatization detection method is improved, the derivatization process introduces additional chemical components, the process is complicated, and is influenced by the conversion rate, and the detection system has poor applicability. Patent CN112858507A discloses an analytical method for measuring dimethyl sulfate in pyraclostrobin by gas chromatography-mass spectrometry, however, the sensitivity and detection limit of the detection method do not meet the quantitative requirements of drug detection.
Disclosure of Invention
In view of this, the application provides a method for detecting sulfate ester in a drug by gas chromatography-mass spectrometry, and the detection method has the advantages of simplicity and convenience in operation, good accuracy, high sensitivity and strong system applicability.
The specific technical scheme of the application is as follows:
a method for detecting sulfate in a medicament by gas chromatography-mass spectrometry is characterized by comprising the following steps:
s1: dissolving a sample with a first organic solvent and an acid solution, adding a salt solution and a second organic solvent, and oscillating to obtain a sample solution;
s2: respectively injecting the test solution and the reference solution into a gas-mass spectrometer, and detecting the content of the sulfate by adopting an external standard method;
the first organic solvent is selected from acetonitrile and/or methanol;
the second organic solvent is selected from cyclohexane and/or n-hexane;
the acid solution is selected from one or more of hydrochloric acid, sulfuric acid and nitric acid;
the salt is selected from one or more of sodium chloride, sodium sulfate, sodium carbonate, sodium bicarbonate and sodium dihydrogen phosphate.
Preferably, the concentration of the acid solution is 1-1.5 mol/L, more preferably 1.2 mol/L, and the volume ratio of the first organic solvent to the acid solution is 1: 1-3, more preferably 1: 2.
Preferably, the concentration of the salt solution is 0.3-0.6 g/mL, more preferably 0.5g/mL, and the volume ratio of the salt solution to the second organic solvent is 1: 1-5, more preferably 1: 3.
Preferably, the volume ratio of the first organic solvent, the acid solution, the salt solution and the second organic solvent is 0.5:1:1: 3.
Preferably, the first organic solvent is selected from acetonitrile, the second organic solvent is selected from cyclohexane, the acid solution is selected from hydrochloric acid, and the salt is selected from sodium sulfate.
Preferably, the concentration of the test solution is 0.02-0.05 mg/mL, and the concentration of the control solution is 10-110 ng/mL.
Preferably, the gas chromatography conditions are: chromatographic column VF-624ms, 30m × 0.25mm × 1.4 μm; carrier gas: he; the temperature of a sample inlet is 180-220 ℃, and more preferably 220 ℃; the flow rate is 1-2 ml/min, and more preferably 1 ml/min; the sample injection volume is 1-2 mu L, and more preferably 1 mu L; the split ratio is 1-5: 1, and the preferable ratio is 4: 1.
Preferably, the column temperature increasing program of the gas chromatography is as follows: taking 63-77 ℃ as an initial column temperature, heating to 170-190 ℃, keeping for 3-5 min, then heating to 220-250 ℃, and keeping for 1-2 min. More preferably, the column temperature is increased to 180 ℃ at 35 ℃/min and maintained for 4min, and then increased to 240 ℃ at 80 ℃/min and maintained for 2min, starting at 70 ℃.
Preferably, the mass spectrometry conditions are: collecting type MRM; an ion source EI; the ion source temperature is 230-250 ℃, and more preferably 250 ℃; the monitoring ion pair includes 66/48 and/or 139/59.
Preferably, the medicament comprises dexrazoxane and the sulphate ester comprises dimethyl sulphate and/or diethyl sulphate.
In summary, the present application provides a method for GC-MS detection of sulfate in a drug. The method comprises the steps of dissolving a test sample by using a first organic solvent and an acid solution, adjusting the ionic strength by using a salt solution and a second organic solvent, carrying out liquid-liquid extraction, and detecting the content of sulfate compounds in the obtained test sample solution by using a gas chromatograph-mass spectrometer. The detection method is simple and convenient to operate, consumes less time, is verified by methodology, has good specificity, linearity, accuracy, sensitivity and stability, and meets the requirement of measuring the content of sulfate compounds in the medicine.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings needed to be used in the description of the embodiments or the prior art will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present application, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without inventive exercise.
FIG. 1 is a spectrum of dimethyl sulfate for group 1 of example 1 herein;
FIG. 2 is a spectrum of diethyl sulfate for group 1 in example 1 of the present application;
FIG. 3 is a spectrum of dimethyl sulfate for group 2 of example 1 herein;
FIG. 4 is a spectrum of diethyl sulfate for group 2 in example 1 of the present application;
FIG. 5 is a spectrum of dimethyl sulfate for group 3 in example 1 of the present application;
FIG. 6 is a diethyl sulfate pattern for group 3 in example 1 of the present application;
FIG. 7 is a spectrum of dimethyl sulfate for group 4 in example 1 of the present application;
FIG. 8 is a diethyl sulfate pattern for group 4 in example 1 of the present application;
FIG. 9 is a verification map of the specificity in example 3 of the present application;
FIG. 10 is a linear regression curve of dimethyl sulfate in example 3 of the present application;
FIG. 11 is a linear regression curve of diethyl sulfate in example 3 of the present application.
Detailed Description
In order to make the objects, features and advantages of the present application more obvious and understandable, the technical solutions in the embodiments of the present application are clearly and completely described, and it is obvious that the embodiments described below are only a part of the embodiments of the present application, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
The raw materials and reagents used in the examples of the present application are commercially available or self-made.
Solution formulation in the examples of the present application:
hydrochloric acid solution: precisely measuring 5ml of hydrochloric Acid (AR), placing the solution in a 50ml volumetric flask, and adding ultrapure water to dilute the solution to scale.
Sodium sulfate solution: 60g of anhydrous sodium sulfate (AR) is weighed, 100ml of ultrapure water is added, ultrasonic treatment is carried out for 10min, and shaking is carried out uniformly.
Example 1
This example was developed for the parameter setting conditions of gas chromatography:
1. sample solution: accurately weighing 10mg of dimethyl sulfate and diethyl sulfate respectively, placing the dimethyl sulfate and the diethyl sulfate into a 10ml volumetric flask, adding acetonitrile to dissolve and dilute the dimethyl sulfate and the diethyl sulfate to a scale, after gradient dilution, taking 0.5ml to a 15ml centrifugal tube, adding 5ml of acetonitrile, carrying out vortex oscillation for 1min, standing for layering, taking supernate and filtering to obtain a mixed reference solution with the concentration of 50 ng/ml.
2. Gas chromatography conditions: carrier gas: he; the flow rate is 1.00 ml/min; the sample injection volume is 1 mu L; the temperature of a sample inlet is 220 ℃; the remaining parameter settings are shown in table 1 below.
TABLE 1
3. The mass spectrum conditions are as follows: collecting type MRM; an ion source EI; delaying the solvent for 3 min; the ion source temperature is 250 ℃; the transmission line temperature is 240 ℃; the temperature of a quadrupole rod MS1 is 150 ℃; the temperature of a quadrupole rod MS2 is 150 ℃;
scanning parameters are as follows: dimethyl sulfate: 66/48, CE 15 (eV); 96/65, CE 15 (eV); 96 → 48, CE 50 (eV);
diethyl sulfate: 139/59, CE 3 (eV); 139/41, CE 3 (eV); 111/81, CE 25 (eV); 111/64, CE 45 (eV).
And drawing a map by taking the acquisition time (min) as an abscissa and the response value as an ordinate. The spectrum of dimethyl sulfate in group 1 is shown in fig. 1, the spectrum of diethyl sulfate in group 1 is shown in fig. 2, the spectrum of dimethyl sulfate in group 2 is shown in fig. 3, the spectrum of diethyl sulfate in group 2 is shown in fig. 4, the spectrum of dimethyl sulfate in group 3 is shown in fig. 5, the spectrum of diethyl sulfate in group 3 is shown in fig. 6, the spectrum of dimethyl sulfate in group 4 is shown in fig. 7, and the spectrum of diethyl sulfate in group 4 is shown in fig. 8.
The experimental results show that the three ion peak shapes of the dimethyl sulfate in the group 1 are all trailing; diethyl sulfate had significant interference with three qualitative ions other than 139/59 (fig. 1 and 2). After the chromatographic column of the group 2 is unchanged, the split ratio is adjusted, and the temperature rise program is carried out, the tailing and the signal-to-noise ratio of three ion peak shapes of the dimethyl sulfate still exist, and the detection limit is not up to 3 ppb; all four ions of diethyl sulfate have interference and poor response (fig. 3 and 4). After the chromatographic column of the group 3 is replaced on the basis of the group 1, the peak time of the dimethyl sulfate is 4.907min, wherein except that the base line of 96/65 is higher, the other two ion peaks have good shapes, but the signal-to-noise ratio cannot meet the requirement; the peak-off time of diethyl sulfate was 6.063min, wherein 111/81 ions did not peak, the ion peaks were worse than 139/59, and the signal-to-noise ratio was not satisfactory (fig. 5 and 6). In group 4, on the basis of group 3, after the split ratio and the temperature rise program are adjusted, the signal-to-noise ratios of dimethyl sulfate and diethyl sulfate are both greater than 3, and the detection requirements are met (fig. 7 and 8).
Example 2
This example was developed for a solution processing method:
referring to the detection method of example 1, wherein the gas chromatography conditions in step 2 are set with the parameters of group 4, the only difference is that the sample solution treatment method in step 1 is: accurately weighing 0.2g of dexrazoxane raw material medicine, placing in a 15ml centrifuge tube, adding 0.5ml of mixed reference substance solution with the concentration of 300 ng/ml after gradient dilution and acid solution for dissolving, adding different solutions for extraction, performing vortex oscillation for 1min, standing for layering, taking supernatant, and filtering to obtain the dexrazoxane raw material medicine.
The recovery rate was measured by loading the sample solution, and the kind, amount and average recovery rate of the solution used in this example were as shown in Table 2 below, and measured 6 times in succession.
TABLE 2
The experimental results show that the recovery rates of dimethyl sulfate and diethyl sulfate in group 5 are not qualified. After the amount of formic acid in the group 6 was increased based on the group 5, the recovery rate of 6 consecutive needles gradually decreased, and the stability and the repeatability were not in compliance with the regulations. Group 7, after extraction with cyclohexane on a group 6 basis, showed too small a response to be detected, probably because dimethyl sulfate and diethyl sulfate were mainly dissolved in formic acid, and it was difficult for cyclohexane to extract dimethyl sulfate and diethyl sulfate from the formic acid layer. In the group 8, after the saturated sodium carbonate is added on the basis of the group 7 for neutralization, the recovery rate of dimethyl sulfate is poor, the reaction of the sodium carbonate and formic acid is severe, and the solution has the risk of flushing out of a centrifugal tube. Group 9 was detected by changing formic acid to hydrochloric acid and adding saturated sodium chloride to the mixture of group 7, but the recovery rate of dimethyl sulfate was not satisfactory. Group 10 improved but still not ideal recovery of dimethyl sulfate after replacing saturated sodium chloride with sodium sulfate solution on the basis of group 9. In group 11, on the basis of group 10, after the water phase is reduced and the organic phase is increased, the recovery rates of dimethyl sulfate and diethyl sulfate reach the standard and the precision is good.
Example 3
In this embodiment, which is a verification of the detection method, the experimental operation steps are as follows:
1. control solution: accurately weighing 10mg of dimethyl sulfate and diethyl sulfate respectively, placing the dimethyl sulfate and the diethyl sulfate into a 10ml volumetric flask, adding acetonitrile to dissolve and dilute the dimethyl sulfate and the diethyl sulfate to a scale, after gradient dilution, respectively taking 0.5ml of the solution into different 15ml centrifugal tubes, adding 1ml of hydrochloric acid solution and 1ml of sodium sulfate solution, accurately adding 3ml of cyclohexane solution, carrying out vortex oscillation for 1min, standing for layering, taking supernatant, and filtering to obtain a standard curve solution with the concentration of 5.09-103.85 ng/ml.
2. Test solution: accurately weighing 0.2g of dexrazoxane raw material medicine, placing in a 15ml centrifuge tube, adding 0.5ml acetonitrile and 1ml hydrochloric acid solution, performing vortex oscillation to dissolve, sequentially adding 1ml sodium sulfate solution and 3ml cyclohexane solution, performing vortex oscillation for 1min, standing for layering, and filtering supernatant to obtain the dexrazoxane raw material medicine.
3. Adding a standard solution: accurately weighing 0.2g of dexrazoxane raw material medicine, placing the dexrazoxane raw material medicine into a 15ml centrifuge tube, adding 0.5ml of reference substance solution with the concentration of 300 ng/ml and 1ml of hydrochloric acid solution after gradient dilution for dissolving, adding 1ml of sodium sulfate solution and 3ml of cyclohexane solution, performing vortex oscillation for 1min, standing for layering, taking supernatant, and filtering to obtain the labeling solution.
4. Gas chromatography conditions: chromatographic column VF-624ms, 30m × 0.25mm × 1.4 μm; carrier gas: he; the temperature of a sample inlet is 220 ℃; the flow rate is 1.00 ml/min; the sample injection volume is 1 mu L; the split ratio is 4: 1;
temperature rising procedure: taking 70 deg.C as initial column temperature, heating to 180 deg.C at 35 deg.C/min, holding for 4min, heating to 240 deg.C at 80 deg.C/min, and holding for 2 min.
5. The mass spectrum conditions are as follows: collecting type MRM; an ion source EI; delaying the solvent for 3 min; the ion source temperature is 250 ℃; the transmission line temperature is 240 ℃; the temperature of a quadrupole rod MS1 is 150 ℃; the temperature of a quadrupole rod MS2 is 150 ℃;
scanning parameters are as follows: dimethyl sulfate: 66/48, CE 15 (eV); diethyl sulfate: 139/59, CE 3 (eV).
The experimental results are as follows:
1. the specificity is as follows:
and (3) sampling and detecting the standard solution, wherein the atlas is shown in figure 9, and each target peak in the figure has no obvious interference, which indicates that the specificity of the method is good.
2. Linearity and range:
the standard curve solution is subjected to sample loading detection, as shown in fig. 10, the result shows that in the range of 10.39 ng/ml-103.85 ng/ml, the peak area of dimethyl sulfate and the concentration form a good linear relation, the correlation coefficient r is not less than 0.990, and the ratio of the absolute value of the y-axis intercept to the 100% limit concentration response value is 5.7%. As shown in FIG. 11, in the range of 10.18ng/ml to 101.79ng/ml, the peak area of diethyl sulfate and the concentration have good linear relationship, the correlation coefficient r is not less than 0.990, and the ratio of the absolute value of y-axis intercept and the response value of 100% limit concentration is 0.7%, which indicates that the method is linear and in accordance with the regulations.
3. Detection limit and quantitation limit:
the sample is respectively loaded with a control solution with the concentration of 5ng/ml (the limit concentration is 10 percent) and a control solution with the concentration of 10ng/ml (the limit concentration is 20 percent), and the sample is continuously injected for 3 times and 6 times respectively for analysis.
The result shows that the control solution with 10% detection limit concentration of 3 continuous needles, wherein the S/N of dimethyl sulfate is within the range of 7.7-12.9, and the S/N of diethyl sulfate is within the range of 16.5-33.7. 6 continuous reference substance solutions with 20% detection limit concentration are adopted, wherein the S/N ratio of dimethyl sulfate is within 11.1-138.6, the RSD of the peak area is 4.4%, the S/N ratio of diethyl sulfate is within 29.3-233.2, and the RSD of the peak area is 7.4%. The detection limit of dimethyl sulfate is 5.19ng/ml, namely 0.078ppm (mu g/g), and the detection limit of diethyl sulfate is 5.09ng/ml, namely 0.077ppm (mu g/g), indicating that the detection limit and the quantification limit result of the method meet the requirements.
4. Accuracy:
the detection results of dimethyl sulfate and diethyl sulfate are shown in the following tables 3 and 4 respectively, and the results show that the recovery rate of dimethyl sulfate ranges from 87.1% to 99.4%, the recovery rate of diethyl sulfate ranges from 99.9% to 114.8%, and the accuracy result of the method meets the specification.
TABLE 3
TABLE 4
5. Stability:
respectively placing a test solution, a reference solution with the concentration of 50ng/ml and a standard solution at room temperature for different time, and respectively injecting samples for 1 time for detection, wherein detection results are respectively shown in tables 5-7 below.
The result shows that the sample is placed for 26 hours at room temperature, and (1) no dimethyl sulfate or diethyl sulfate is detected in the sample solution; (2) the ratio of the detection concentration of dimethyl sulfate in the 100% limit concentration reference solution to the initial (0 h) detection concentration is 93.6-99.2%, and the ratio of the detection concentration of diethyl sulfate to the initial (0 h) detection concentration is 98.4-106.5%; (3) the ratio of the detection concentration of dimethyl sulfate in the standard solution with 100% limit concentration to the initial (0 h) detection concentration is 91.7-100.1%, and the ratio of the detection concentration of diethyl sulfate to the initial (0 h) detection concentration is 98.3-103.0%. Therefore, the test solution, the 100% limit concentration control solution and the 100% limit concentration standard solution are stable for at least 26 hours at room temperature, and the method has good stability.
TABLE 5
TABLE 6
TABLE 7
The above embodiments are only used for illustrating the technical solutions of the present application, and not for limiting the same; although the present application has been described in detail with reference to the foregoing embodiments, it should be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions in the embodiments of the present application.
Claims (5)
1. A method for detecting sulfate in a medicament by gas chromatography-mass spectrometry is characterized by comprising the following steps:
s1: dissolving a sample with a first organic solvent and an acid solution, adding a salt solution and a second organic solvent, and oscillating to obtain a sample solution;
s2: respectively injecting the test solution and the reference solution into a gas-mass spectrometer, and detecting the content of the sulfate by adopting an external standard method;
the first organic solvent is selected from acetonitrile, the second organic solvent is selected from cyclohexane, the acid solution is selected from hydrochloric acid, the salt is selected from sodium sulfate, and the volume ratio of the first organic solvent, the acid solution, the salt solution and the second organic solvent is 0.5:1:1: 3;
the gas chromatography conditions were: chromatographic column VF-624ms, 30m × 0.25mm × 1.4 μm; carrier gas: he; the temperature of a sample inlet is 220 ℃; the flow rate is 1 ml/min; the sample injection volume is 1 mu L; the split ratio is 4: 1;
the column temperature heating program of the gas chromatography is as follows: taking 70 deg.C as initial column temperature, heating to 190 deg.C, maintaining for 3min, heating to 220 deg.C, and maintaining for 1 min;
the drug is dexrazoxane, and the sulfate is dimethyl sulfate and/or diethyl sulfate.
2. The method for detecting sulfate ester in a drug by gas chromatography-mass spectrometry according to claim 1, wherein the concentration of the acid solution is 1-1.5 mol/L.
3. The method for detecting sulfate ester in a drug by gas chromatography-mass spectrometry of claim 1, wherein the concentration of the salt solution is 0.3-0.6 g/mL.
4. The method for detecting sulfate ester in a drug by gas chromatography-mass spectrometry according to claim 1, wherein the concentration of the test solution is 0.02-0.05 mg/mL, and the concentration of the control solution is 10-110 ng/mL.
5. The GC-MS method of claim 1, wherein the mass spectrometry conditions are as follows: collecting type MRM; an ion source EI; the temperature of the ion source is 230-250 ℃; the monitoring ion pair includes 66/48 and/or 139/59.
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Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6787366B1 (en) * | 1996-12-11 | 2004-09-07 | The United States Of America As Represented By The Secretary Of The Army | Microspot test kit and method for chemical testing |
| CN101620210A (en) * | 2009-08-12 | 2010-01-06 | 西北师范大学 | Method for rapidly detecting sulphur content in polysaccharide sulfate |
| CN104280490A (en) * | 2013-07-02 | 2015-01-14 | 南通中国科学院海洋研究所海洋科学与技术研究发展中心 | Quality analysis method of brown algae polysaccharide sulfate |
| CN107422112A (en) * | 2017-07-01 | 2017-12-01 | 河南科技大学 | A kind of immune reagent kit for detecting ethopabate, preparation method and application |
| WO2018107975A1 (en) * | 2016-12-13 | 2018-06-21 | 江苏奥赛康药业股份有限公司 | Dexrazoxane analysis method |
| CN111579689A (en) * | 2020-06-11 | 2020-08-25 | 江苏联环药业股份有限公司 | Method for measuring content of dimethyl sulfate in clopidogrel hydrogen sulfate |
| CN112710762A (en) * | 2020-12-25 | 2021-04-27 | 北京金城泰尔制药有限公司 | Method for measuring residual quantity of dimethyl sulfate |
| CN112858507A (en) * | 2021-01-12 | 2021-05-28 | 苏州国辰生物科技股份有限公司 | Analysis method for measuring dimethyl sulfate in pyraclostrobin by gas chromatography-mass spectrometry |
| CN113382997A (en) * | 2019-01-31 | 2021-09-10 | 拜耳股份有限公司 | Monohydrate of hydrochloric acid Rogatinib and solid state thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111413440A (en) * | 2020-05-06 | 2020-07-14 | 上海臣邦医药科技股份有限公司 | Method for detecting parecoxib sodium sulfate genotoxic impurities |
-
2021
- 2021-09-08 CN CN202111030420.0A patent/CN113720956B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6787366B1 (en) * | 1996-12-11 | 2004-09-07 | The United States Of America As Represented By The Secretary Of The Army | Microspot test kit and method for chemical testing |
| CN101620210A (en) * | 2009-08-12 | 2010-01-06 | 西北师范大学 | Method for rapidly detecting sulphur content in polysaccharide sulfate |
| CN104280490A (en) * | 2013-07-02 | 2015-01-14 | 南通中国科学院海洋研究所海洋科学与技术研究发展中心 | Quality analysis method of brown algae polysaccharide sulfate |
| WO2018107975A1 (en) * | 2016-12-13 | 2018-06-21 | 江苏奥赛康药业股份有限公司 | Dexrazoxane analysis method |
| CN107422112A (en) * | 2017-07-01 | 2017-12-01 | 河南科技大学 | A kind of immune reagent kit for detecting ethopabate, preparation method and application |
| CN113382997A (en) * | 2019-01-31 | 2021-09-10 | 拜耳股份有限公司 | Monohydrate of hydrochloric acid Rogatinib and solid state thereof |
| CN111579689A (en) * | 2020-06-11 | 2020-08-25 | 江苏联环药业股份有限公司 | Method for measuring content of dimethyl sulfate in clopidogrel hydrogen sulfate |
| CN112710762A (en) * | 2020-12-25 | 2021-04-27 | 北京金城泰尔制药有限公司 | Method for measuring residual quantity of dimethyl sulfate |
| CN112858507A (en) * | 2021-01-12 | 2021-05-28 | 苏州国辰生物科技股份有限公司 | Analysis method for measuring dimethyl sulfate in pyraclostrobin by gas chromatography-mass spectrometry |
Non-Patent Citations (4)
| Title |
|---|
| HIGH PERFORMANCE LIQUID CHROMATOGRAPHIC ANALYSIS OF THE CARDIOPROTECTIVE AGENT DEXRAZOXANE IN HUMAN PLASMA AND URINE;H. Rosing 等;《J. LIQ. CHROM. & REL. TECHNOL.》;19971231;第20卷(第4期);第583-601页 * |
| 工作场所空气中硫酸二甲酯的气相色谱质谱分析方法研究;高亚利 等;《工业卫生与职业病》;20171231;第43卷(第5期);第383-385页 * |
| 气相色谱-质谱联用法测定纺织品中硫酸二甲酯和硫酸二乙酯;裴德君;《分析试验室》;20150131;第34卷(第1期);第31-34页 * |
| 气相色谱－质谱联用测定化妆品中硫酸二甲酯与硫酸二乙酯;吴楚森 等;《分析测试学报》;20180131;第37卷(第1期);第70-75页 * |
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