CN103197002A - Detection method of ethylene oxide and dioxane residue contents in polyethylene glycol 4000 - Google Patents
Detection method of ethylene oxide and dioxane residue contents in polyethylene glycol 4000 Download PDFInfo
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- CN103197002A CN103197002A CN2012100007139A CN201210000713A CN103197002A CN 103197002 A CN103197002 A CN 103197002A CN 2012100007139 A CN2012100007139 A CN 2012100007139A CN 201210000713 A CN201210000713 A CN 201210000713A CN 103197002 A CN103197002 A CN 103197002A
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Abstract
The invention relates to a detection method of impurities in a polymer, and specifically relates to a detection method of ethylene oxide and dioxane residue contents in polyethylene glycol 4000.
Description
Technical field:
The present invention relates to the method for detecting impurities in a kind of polymkeric substance, particularly the detection method of the residuals content of oxirane and dioxane in a kind of Macrogol 4000.
Background technology:
Macrogol 4000 (being called for short PEG4000) is the potpourri that oxirane and water polycondensation form.PEG4000 is used as matrix in medicine, cosmetics industry in producing, and works to regulate viscosity, fusing point; In rubber, metal-processing industry, be used as lubricant, cooling medium, in agricultural chemicals, pigment industry production, be used as spreading agent, emulsifying agent; In textile industry, be used as antistatic agent, lubricant etc.Of many uses, market outlook are big.Product can be divided into several series such as pharmaceutical grade, cosmetics-stage, food-grade and technical grade.Pharmaceutical grade PEG4000 price if as seen buy technical grade PEG4000, by refining means, obtains to reach the product that pharmaceutical grade requires, remarkable in economical benefits far above technical grade PEG4000.Reason owing to security and environmental protection aspect, control has higher requirement to pharmacopeia to organic solvent residue amount wherein, and pharmaceutical grade PEG4000 must meet the pharmacopeia requirement, therefore must control the Determination of Residual Organic Solvents that PEG4000 introduces in process of production.Therefore PEG4000 exists the possibility that contains residual solvent oxirane and dioxane owing to used oxirane and dioxane in production run and the purge process, is necessary oxirane and dioxane detection method are studied.Existing method complicated operation, sensitivity is not high, therefore needs to improve, to be conducive to the quality control to medicine.
The present invention adopts the content of oxirane and dioxane in the Headspace Gas Chromatography Macrogol 4000, and method is easy, and is highly sensitive, and the result accurately and reliably.
Summary of the invention:
What the present invention relates to is the detection method of oxirane and dioxane residuals content in the Macrogol 4000.
Method of the present invention, the process following steps:
Step 1, the preparation of oxirane reference substance solution;
Step 2, the preparation of dioxane reference substance solution;
Step 3, the need testing solution preparation;
Step 4 adds the preparation of standard specimen need testing solution;
Step 5, inject gas chromatograph obtains chromatogram;
Step 6 is calculated oxirane and dioxane residuals content in the test sample.
Wherein, the method for step 1 is as follows:
Under the low temperature environment, precision is measured oxirane standard solution 1ml and is put in the 100ml measuring bottle that contains the 50ml PEG400, adds same solvent and is diluted to scale, shake up oxirane reference substance storing solution; Precision is measured oxirane reference substance storing solution 200 μ l and is put in the 10ml measuring bottle that contains 3ml two pure water, adds two pure water and is diluted to scale, shakes up.
The method of step 2 is as follows:
It is an amount of to get the dioxane reference substance, and accurate the title decides, and water is made the reference substance solution that concentration is 80 μ g/ml.The method of step 3 is as follows:
The about 1g of taking polyethylene glycol 400 test samples, the accurate title, decide, and places the head space bottle, adds two pure water 1ml, and sealing shakes up.
The method of step 4 is as follows:
The about 1g of taking polyethylene glycol 400 test samples, the accurate title, decide, and places the head space bottle, adds 0.5ml oxirane reference substance solution and 0.5ml dioxane solution, and sealing shakes up.
The chromatographic condition of step 5 is as follows:
Head space condition head space heating-up temperature: 90 ℃; Heat time heating time: 30min; Injection annulus temperature: 95 ℃; Delivery pipe temperature: 100 ℃; Jolt intensity for strong, jolt 1min; Sampling volume is head space bottle upper gas 1ml, automatically headspace sampling.
Chromatographic condition Angilent HP-INNOWAX capillary column (60.0m * 0.32mm * 0.5 μ m), 200 ℃ of injector temperatures, 250 ℃ of detector temperatures, initial temperature is 35 ℃, kept 5 minutes, speed with 5 ℃/min rises to 180 ℃ again, and the speed with 30 ℃/min rises to 230 ℃ again, keeps 5min; Split ratio 20: 1, carrier gas are nitrogen, flow velocity 0.4ml/min.
The present invention adopts calibration curve method that oxirane in the test sample and dioxane residuals content are measured, described calibration curve method is that the standard reference material with variable concentrations carries out peak area and measures, be that ordinate reference substance concentration is horizontal ordinate with the peak area, draw a typical curve, by the peak area of oxirane and dioxane in the mensuration test sample, calculate the content of corresponding oxirane and dioxane residue.
The drafting of typical curve of the present invention is as follows:
Accurate absorption dioxane reference substance storing solution (0.32mg/ml) 2,5,10,20,50mL put respectively in the 100mL measuring bottle, under low temperature environment, add oxirane reference substance storing solution 0.25,0.5,1,2,4ml more successively, add two pure water and be diluted to scale, shake up.Precision is measured 1mL respectively, puts in the 10mL head space bottle, and is airtight, measure in accordance with the law, and be ordinate (Y) with the reference substance solution peak area, reference substance solution concentration is horizontal ordinate (X), carries out linear regression, regression equation and the range of linearity see Table 1.
Table 1 regression equation and the range of linearity (n=6)
Detection method of the present invention obtains through screening, and screening process is as follows
1 instrument and reagent
Agilent 6890N gas chromatograph, Agilent 7694E headspace sampling instrument, fid detector; Analytical balance (the plum Teller-Tuo benefit XS105DU of Instr Ltd.); Miniature whirlpool mixed instrument (Shanghai Hu Xi analytical instrument Co., Ltd., Factory); Two pure water (self-control); Oxirane (lot number: 4-8891, SEPELCO); Dioxane (lot number: 19381, CHEM SERVICE); PEG4000 (Tianjin Bokelin Medicine Packaging Technology Co., Ltd.).
2 methods and result
2.1 head space condition head space heating-up temperature: 90 ℃; Heat time heating time: 30min; Injection annulus temperature: 95 ℃; Delivery pipe temperature: 100 ℃; Jolt intensity for strong, jolt 1min; Sampling volume is head space bottle upper gas 1ml, automatically headspace sampling.
2.2 chromatographic condition Angilent HP-INNOWAX capillary column (60.0m * 0.32mm * 0.5 μ m), 200 ℃ of injector temperatures, 250 ℃ of detector temperatures, initial temperature is 35 ℃, kept 5 minutes, speed with 5 ℃/min rises to 180 ℃ again, and the speed with 30 ℃/min rises to 230 ℃ again, keeps 5min; Split ratio 20: 1, carrier gas are nitrogen, flow velocity 0.4ml/min.
2.3 the preparation of solution
2.3.1 oxirane reference substance solution preparation: under the low temperature environment, precision is measured oxirane standard solution 1ml and is put in the 100ml measuring bottle that contains the 50ml PEG400, adds same solvent and is diluted to scale, shake up oxirane reference substance storing solution; Precision is measured oxirane reference substance storing solution 200 μ l and is put in the 10ml measuring bottle that contains 3ml two pure water, adds two pure water and is diluted to scale, shakes up.
2.3.2 the preparation of dioxane reference substance solution: it is an amount of to get the dioxane reference substance, the accurate title, decide, and water is made the reference substance solution that concentration is 80 μ g/ml.
2.3.3 need testing solution preparation: get the about 1g of test sample, the accurate title, decide, and places the head space bottle, adds two pure water 1ml, and sealing shakes up.
2.3.4 add the standard specimen need testing solution: get the about 1g of test sample, the accurate title, decide, and places the head space bottle, adds 0.5ml oxirane reference substance solution and 0.5ml dioxane solution, and sealing shakes up.
2.4 the drafting of typical curve accurate absorption dioxane reference substance storing solution (0.32mg/ml) 2,5,10,20,50mL put respectively in the 100mL measuring bottle, under low temperature environment, add oxirane reference substance storing solution 0.25,0.5,1,2,4ml more successively, add two pure water and be diluted to scale, shake up.Precision is measured 1mL respectively, puts in the 10mL head space bottle, and is airtight, measure in accordance with the law, and be ordinate (Y) with the reference substance solution peak area, reference substance solution concentration is horizontal ordinate (X), carries out linear regression, regression equation and the range of linearity see Table 1.
Table 1 regression equation and the range of linearity (n=6)
2.5 computing method computing formula: (standard addition method)
c
xConcentration (μ g/ml) for component x in the test sample; Ax is the chromatographic peak area of component x in the test sample; Δ c
xConcentration (μ g/ml) for the component reference substance to be measured of the concentration known that adds; A
IsChromatographic peak area for component x behind the adding reference substance; V is sample solution volume (ml); W is the quality (g) of test sample.
2.6 precision is tested respectively, and precision is measured the oxirane reference substance solution and dioxane reference substance solution 5mL puts in the 10mL measuring bottle, as mixing reference substance solution.Precision is measured 5 parts of reference substance solution, and every part of 1mL puts in the 10mL head space bottle, and is airtight, shakes up, and measures with method, and the RSD of ring oxidative ethane and dioxane peak area is respectively 2.8%, 2.3%.
2.7 the replica test precision takes by weighing 5 parts of same batch samples, every part of about 1G puts in the 10mL head space bottle, adds 1mL water, and is airtight, shakes up.Measure with method, calculate content according to standard addition method, the RSD of ring oxidative ethane and dioxane content is respectively 2.2%, 1.1%.
2.8 the recovery test precision is measured mixing reference substance solution 20,25,30mL puts respectively in the 100mL measuring bottle, thin up is to scale.Precision takes by weighing 9 parts of test sample (known solvent content) solution, and every part of 0.2g puts in the 10mL head space bottle, and the reference substance solution 1mL of the above-mentioned 3 kinds of concentration of the accurate adding of difference (each 3 parts, n=9) airtight, shake up.Measure with method, calculate according to standard addition method, the results are shown in Table 2.
Table 2 recovery test
2.9 sample determination result accurate title respectively decides test sample 1g, presses need testing solution preparation method preparation, above-mentioned chromatographic condition detects, and calculates with the standard solution addition method, averages as measurement result, the results are shown in Table 3.
Table 3 sample determination result
3 discuss
This research has been compared DB-17, HP-FFAP, these three kinds of different chromatographic columns of HP-INNOWAX to the influence of the separating effect of oxirane and dioxane, and the result shows that both separating effects on the HP-INNOWAX chromatographic column are best.Analyzing reason may be that oxirane and dioxane polarity are stronger, thereby can obtain good separation on the HP-INNOWAX chromatographic column of strong polarity.
Embodiment:
Further specify the present invention by the following examples, but not as limitation of the present invention.
Embodiment 1
Method of the present invention, the process following steps:
Step 1, the preparation of oxirane reference substance solution;
Step 2, the preparation of dioxane reference substance solution;
Step 3, the need testing solution preparation;
Step 4 adds the preparation of standard specimen need testing solution;
Step 5, inject gas chromatograph obtains chromatogram;
Step 6 is calculated oxirane and dioxane residuals content in the test sample.
Wherein, the method for step 1 is as follows:
Under the low temperature environment, precision is measured oxirane standard solution 1ml and is put in the 100ml measuring bottle that contains the 50ml PEG400, adds same solvent and is diluted to scale, shake up oxirane reference substance storing solution; Precision is measured oxirane reference substance storing solution 200 μ l and is put in the 10ml measuring bottle that contains 3ml two pure water, adds two pure water and is diluted to scale, shakes up.
The method of step 2 is as follows:
It is an amount of to get the dioxane reference substance, and accurate the title decides, and water is made the reference substance solution that concentration is 80 μ g/ml.The method of step 3 is as follows:
Get the about 1g of test sample, the accurate title, decide, and places the head space bottle, adds two pure water 1ml, and sealing shakes up.
The method of step 4 is as follows:
Get the about 1g of test sample, the accurate title, decide, and places the head space bottle, adds 0.5ml oxirane reference substance solution and 0.5ml dioxane solution, and sealing shakes up.
The chromatographic condition of step 5 is as follows:
Head space condition head space heating-up temperature: 90 ℃; Heat time heating time: 30min; Injection annulus temperature: 95 ℃; Delivery pipe temperature: 100 ℃; Jolt intensity for strong, jolt 1min; Sampling volume is head space bottle upper gas 1ml, automatically headspace sampling.
Chromatographic condition Angilent HP-INNOWAX capillary column (60.0m * 0.32mm * 0.5 μ m), 200 ℃ of injector temperatures, 250 ℃ of detector temperatures, initial temperature is 35 ℃, kept 5 minutes, speed with 5 ℃/min rises to 180 ℃ again, and the speed with 30 ℃/min rises to 230 ℃ again, keeps 5min; Split ratio 20: 1, carrier gas are nitrogen, flow velocity 0.4ml/min.
The drafting of typical curve is as follows:
Accurate absorption dioxane reference substance storing solution (0.32mg/ml) 2,5,10,20,50mL put respectively in the 100mL measuring bottle, under low temperature environment, add oxirane reference substance storing solution 0.25,0.5,1,2,4ml more successively, add two pure water and be diluted to scale, shake up.Precision is measured 1mL respectively, puts in the 10mL head space bottle, and is airtight, measure in accordance with the law, and be ordinate (Y) with the reference substance solution peak area, reference substance solution concentration is horizontal ordinate (X), carries out linear regression, regression equation and the range of linearity see Table 1.
Table 1 regression equation and the range of linearity (n=6)
Claims (8)
1. the detection method of the residuals content of oxirane and dioxane in the Macrogol 4000 is characterized in that, comprises the steps:
Step 1, the preparation of oxirane reference substance solution;
Step 2, the preparation of dioxane reference substance solution;
Step 3, the need testing solution preparation;
Step 4 adds the preparation of standard specimen need testing solution;
Step 5, inject gas chromatograph obtains chromatogram;
Step 6 is calculated oxirane and dioxane residuals content in the test sample.
2. according to the detection method of claim 1, it is characterized in that, wherein, the method of step 1 is as follows: under the low temperature environment, precision is measured oxirane standard solution 1ml and is put in the 100ml measuring bottle that contains the 50ml PEG400, adds same solvent and is diluted to scale, shake up oxirane reference substance storing solution; Precision is measured oxirane reference substance storing solution 200 μ l and is put in the 10ml measuring bottle that contains 3ml two pure water, adds two pure water and is diluted to scale, shakes up.
3. according to the detection method of claim 1, it is characterized in that,
The method of step 2 is as follows:
It is an amount of to get the dioxane reference substance, and accurate the title decides, and water is made the reference substance solution that concentration is 80 μ g/ml.
4. according to the detection method of claim 1, it is characterized in that the method for step 3 is as follows:
Get the about 1g of test sample, the accurate title, decide, and places the head space bottle, adds two pure water 1ml, and sealing shakes up.
5. according to the detection method of claim 1, it is characterized in that the method for step 4 is as follows:
Get the about 1g of test sample, the accurate title, decide, and places the head space bottle, adds 0.5ml oxirane reference substance solution and 0.5ml dioxane solution, and sealing shakes up.
6. according to the detection method of claim 1, it is characterized in that the chromatographic condition of step 5 is as follows:
Head space condition head space heating-up temperature: 90 ℃; Heat time heating time: 30min; Injection annulus temperature: 95 ℃; Delivery pipe temperature: 100 ℃; Jolt intensity for strong, jolt 1min; Sampling volume is head space bottle upper gas 1ml, automatically headspace sampling;
Chromatographic condition Angilent HP-INNOWAX capillary column (60.0m * 0.32mm * 0.5 μ m), 200 ℃ of injector temperatures, 250 ℃ of detector temperatures, initial temperature is 35 ℃, kept 5 minutes, speed with 5 ℃/min rises to 180 ℃ again, and the speed with 30 ℃/min rises to 230 ℃ again, keeps 5min; Split ratio 20: 1, carrier gas are nitrogen, flow velocity 0.4ml/min.
7. according to the detection method of claim 1, it is characterized in that the drafting of typical curve is as follows:
Accurate absorption dioxane reference substance storing solution (0.32mg/ml) 2,5,10,20,50mL put respectively in the 100mL measuring bottle, under low temperature environment, add oxirane reference substance storing solution 0.25,0.5,1,2,4ml more successively, add two pure water and be diluted to scale, shake up; Precision is measured 1mL respectively, puts in the 10mL head space bottle, and is airtight, measure in accordance with the law, and be ordinate with the reference substance solution peak area, reference substance solution concentration is horizontal ordinate, carries out linear regression.
8. according to the detection method of claim 1, it is characterized in that, comprise the steps:
Step 1, the preparation of oxirane reference substance solution;
Step 2, the preparation of dioxane reference substance solution;
Step 3, the need testing solution preparation;
Step 4 adds the preparation of standard specimen need testing solution;
Step 5, inject gas chromatograph obtains chromatogram;
Step 6 is calculated oxirane and dioxane residuals content in the test sample;
Wherein, the method for step 1 is as follows:
Under the low temperature environment, precision is measured oxirane standard solution 1ml and is put in the 100ml measuring bottle that contains the 50ml PEG400, adds same solvent and is diluted to scale, shake up oxirane reference substance storing solution; Precision is measured oxirane reference substance storing solution 200 μ l and is put in the 10ml measuring bottle that contains 3ml two pure water, adds two pure water and is diluted to scale, shake up,
The method of step 2 is as follows:
It is an amount of to get the dioxane reference substance, and accurate the title decides, and water is made the reference substance solution that concentration is 80 μ g/ml, and the method for step 3 is as follows:
Get the about 1g of test sample, the accurate title, decide, and places the head space bottle, adds two pure water 1ml, and sealing shakes up, and the method for step 4 is as follows:
Get the about 1g of test sample, the accurate title, decide, and places the head space bottle, adds 0.5ml oxirane reference substance solution and 0.5ml dioxane solution, and sealing shakes up,
The chromatographic condition of step 5 is as follows:
Head space condition head space heating-up temperature: 90 ℃; Heat time heating time: 30min; Injection annulus temperature: 95 ℃; Delivery pipe temperature: 100 ℃; Jolt intensity for strong, jolt 1min; Sampling volume is head space bottle upper gas 1ml, automatic headspace sampling,
Chromatographic condition Angilent HP-INNOWAX capillary column (60.0m * 0.32mm * 0.5 μ m), 200 ℃ of injector temperatures, 250 ℃ of detector temperatures, initial temperature is 35 ℃, kept 5 minutes, speed with 5 ℃/min rises to 180 ℃ again, and the speed with 30 ℃/min rises to 230 ℃ again, keeps 5min; Split ratio 20: 1, carrier gas are nitrogen, flow velocity 0.4ml/min,
The drafting of typical curve is as follows:
Accurate absorption dioxane reference substance storing solution (0.32mg/ml) 2,5,10,20,50mL put respectively in the 100mL measuring bottle, under low temperature environment, add oxirane reference substance storing solution 0.25,0.5,1,2,4ml more successively, add two pure water and be diluted to scale, shake up, precision is measured 1mL respectively, put in the 10mL head space bottle, airtight, measure in accordance with the law, be ordinate with the reference substance solution peak area, reference substance solution concentration is horizontal ordinate, carries out linear regression.
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| CN201210000713.9A CN103197002B (en) | 2012-01-04 | 2012-01-04 | The detection method of the residuals content of a kind of Macrogol 4000 ethylene oxide and dioxane |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106124671A (en) * | 2016-09-19 | 2016-11-16 | 中华人民共和国连云港出入境检验检疫局 | The detection method of residual ethylene oxide in container Sanitation disposal |
| CN106501416A (en) * | 2016-12-09 | 2017-03-15 | 通标标准技术服务(上海)有限公司 | A kind of plastic that determines is with food ethylene oxide and the method for acetaldehyde residual quantity |
| CN106908545A (en) * | 2017-03-23 | 2017-06-30 | 苏州桓晨医疗科技有限公司 | A kind of detection method of minimal residue oxirane |
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| JPS6096605A (en) * | 1983-10-31 | 1985-05-30 | Mitsubishi Chem Ind Ltd | Production of hydrophilic resin |
| WO2000017429A1 (en) * | 1998-09-21 | 2000-03-30 | University Of South Florida | Solid phase microextraction fiber structure and method of making |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106124671A (en) * | 2016-09-19 | 2016-11-16 | 中华人民共和国连云港出入境检验检疫局 | The detection method of residual ethylene oxide in container Sanitation disposal |
| CN106501416A (en) * | 2016-12-09 | 2017-03-15 | 通标标准技术服务(上海)有限公司 | A kind of plastic that determines is with food ethylene oxide and the method for acetaldehyde residual quantity |
| CN106908545A (en) * | 2017-03-23 | 2017-06-30 | 苏州桓晨医疗科技有限公司 | A kind of detection method of minimal residue oxirane |
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Address after: 300410 2 East Road Puji River, Beichen District, Tianjin (Tsun Li modern Chinese medicine city) Patentee after: TASLY PHARMACEUTICAL GROUP Co.,Ltd. Address before: 300410 Tianjin Beichen District Huaihe road and Ting Jiang West Road intersection heaven proud of the park Legal Center Intellectual Property Department Patentee before: TASLY PHARMACEUTICAL GROUP Co.,Ltd. |
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Effective date of registration: 20180719 Address after: No. 3, Ting Jiangxi Road, Beichen District, Tianjin Patentee after: TIANJIN TASLY ST. SPECIALTY PHARMACEUTICAL CO.,LTD. Address before: 300410 2 East Road Puji River, Beichen District, Tianjin (Tsun Li modern Chinese medicine city) Patentee before: TASLY PHARMACEUTICAL GROUP Co.,Ltd. |