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GC-MS法测定甲磺酸萘莫司他原料药中的遗传毒性杂质
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| 篇名： | GC-MS法测定甲磺酸萘莫司他原料药中的遗传毒性杂质 |
| TITLE： | |
| 摘要： | 目的：建立同时测定甲磺酸萘莫司他原料药中遗传毒性杂质甲磺酸甲酯、甲磺酸乙酯、甲磺酸异丙酯的方法。方法：采用气相色谱-质谱联用法，使用二氯甲烷进行提取。色谱柱为DB-5毛细管柱，柱温采用程序升温，进样口温度为240 ℃，柱流量为3.0 ml/min，吹扫流量为6.0 ml/min，进样方式为不分流进样，载气为高纯氦气，检测器为质谱检测器，离子源温度为230 ℃，接口温度为230 ℃，溶剂延迟时间为2.5 min，离子化模式为电子轰击离子化模式，检测器电压为相对于调谐结果，扫描（检测）方式为选择性离子检测，电子能量为70 eV，进样量为1.0 μl。结果：3种杂质成分之间的分离度均＞2.0；3种杂质成分检测质量浓度线性范围均为0.10～20 μg/ml（r≥0.999 5）；精密度、稳定性、重复性试验的RSD＜2％；加样回收率分别为97.7％～104.8％、102.5％～110.7％、103.0％～107.6％，RSD分别为2.8％、2.6％、1.6％（n＝9）。结论：该方法简便、准确、灵敏、迅速，可用于甲磺酸萘莫司他原料药中3种遗传毒性杂质的测定。 |
| ABSTRACT： | OBJECTIVE： To establish a method for determination the genotoxicity impurities （methyl methanesulfonate， ethyl methanesulfonate and isopropyl methanesulfonate） in mesylate nafamostat raw materia. METHODS： GC-MS was conducted， and the genotoxicity impurities were extracted by dichloromethane. The column was DB-5 capillary column by programmed temperature， the inlet temperature was 240 ℃， column flow was 3.0 ml/min， purge flow was 6.0 ml/min， sample mode splitless injection， carrier gas was high purity helium， detector is a mass spectrometer detector， ion source temperature was 230 ℃， the interface temperature was 230 ℃， the delay time of solvent was 2.5 min， ionization mode was electron impact， detector voltage was respect to the tuning results， scanning （detection） method was selective ion monitoring， electron energy was 70 eV， and the injection volume was 1.0 μl. RESULTS： The separation degree of 3 impurities were greater than 2.0； the linear range of 3 impurities were 0.10-20 μg/ml（r≥0.999 5）； RSDs of precision， stability and reproducibility tests were lower than 2％； recoveries were 97.7％-104.8％ （RSD＝2.8％，n＝9），102.5％-110.7％（RSD＝2.6％，n＝9） and 103.0％-107.6％（RSD＝1.6％，n＝9）. CONCLUSIONS： The method is simple， accurate， sensitive and rapid， and can be used for the genotoxicity impurities in mesylate nafamostat raw materia. |
| 期刊： | 2016年第27卷第18期 |
| 作者： | 毛颐晴，李纬，朱丽君 |
| AUTHORS： | MAO Yiqing1，LI wei2，ZHU Lijun |
| 关键字： | 甲磺酸萘莫司他原料药；遗传毒性杂质；甲磺酸甲酯；甲磺酸乙酯；甲磺酸异丙酯；气相色谱-质谱联用法 |
| KEYWORDS： | Mesylate nafamostat raw materia； Genotoxicity impurity； Methyl methanesulfonate； Ethyl methanesulfonate； Isopropyl methanesulfonate； GC-MS |
| 阅读数： | 437 次 |
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