| 引用本文: | 李炎,马旻新,曾实,王叔桥.HS-GC-MS同时测定沙芬酰胺中磺酸酯类基因毒性杂质[J].中国现代应用药学,2019,36(19):2431-2435. |
| LI Yan,MA Minxin,ZENG Shi,WANG Shujiao.Simultaneous Determination of Sulfonate Esters of Genotoxic Impurities in Safinamide by HS-GC-MS[J].Chin J Mod Appl Pharm(中国现代应用药学),2019,36(19):2431-2435. |
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| 摘要: |
| 目的 建立同时测定沙芬酰胺原料药中5种磺酸酯类基因毒性杂质（甲磺酸甲酯、甲磺酸乙酯、甲磺酸异丙酯、甲磺酸丙酯、甲磺酸丁酯）的方法。方法 采用顶空进样气相色谱-质谱联用法，在线衍生，RESTEK Rxi-624Sil毛细管柱（30 m×0.25 mm，1.4 μm），四级杆质量检测器，离子化模式为电子轰击离子化（EI）模式，采集模式为选择离子监测。结果 5种杂质检测限为0.3~1.3 ng·mL-1，定量限为0.9~4.3 ng·mL-1；精密度、稳定性、重复性试验的RSD均<5%；浓度在5~300 ng·mL-1内，5种杂质的峰面积与其相对应的浓度有良好的线性关系，相关系数（r2）均>0.995；回收率为99.4%~100.6%，RSD为0.8%~2.6%（n=9）。结论 该法操作简便，重复性好，结果准确可靠，可用于沙芬酰胺中磺酸酯类基因毒性杂质的测定。 |
| 关键词: 沙芬酰胺 磺酸酯类 基因毒性杂质 顶空进样气相色谱-质谱联用 在线衍生 |
| DOI：10.13748/j.cnki.issn1007-7693.2019.19.013 |
| 分类号:R917.101 |
| 基金项目: |
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| Simultaneous Determination of Sulfonate Esters of Genotoxic Impurities in Safinamide by HS-GC-MS |
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LI Yan, MA Minxin, ZENG Shi, WANG Shujiao
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Sichuan Provincial Institute for Food and Drug Control, Chengdu 611731, China
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| Abstract: |
| OBJECTIVE To establish a simultaneous determination method of five sulfonate esters of genotoxic impurities(methyl methanesulfonate, ethyl methanesulfonate, methanesulfonicacid, 1-methylethylester, propyl methanesulfonate, N-butyl methanesulfonate) in safinamide. METHODS HS-GC-MS with online derivative method was conducted. The column was RESTEK sil Rxi-624 capillary column(30 m×0.25 mm, 1.4 μm). Detector was a mass spectrometer detector, ionization mode was electron impact(EI), collection mode was selection monitoring. RESULTS The detection limit of 5 impurities were 0.3-1.3 ng·mL-1, quantitative limit were 0.9-4.3 ng·mL-1. The RSDs of precision, stability and reproducibility tests were all <5%. Within the concentration range of 5-300 ng·mL-1, the peak area of the 5 impurities had a good linear relationship with the corresponding concentration, and the correlation coefficient (r2) were all >0.995. The recovery rates were 99.4%-100.6% and RSD were 0.8%-2.6%(n=9). CONCLUSION The method is simple, reproducible, accurate, and can be used for the determination of sulfonate esters of genotoxic impurities in safinamide. |
| Key words: safinamide sulfonate esters genotoxic impurities HS-GC-MS online derivation |
