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GC-MS法测定甲磺酸中3种甲磺酸烷基酯类遗传毒性杂质

Determination of genotoxic impurities of alkyl methanesulfonates in methanesulfonic acid by gas chromatography–mass spectrometry

  • 摘要: 建立一种液液萃取GC-MS分析方法,用于测定甲磺酸中遗传毒性杂质甲磺酸甲酯、甲磺酸乙酯、甲磺酸异丙酯。采用甲基聚硅氧烷毛细管色谱柱,程序升温,进样口温度220 ℃,不分流高压进样;质谱正离子模式,选择性监测m/z 56、m/z 79、m/z 80及m/z 123离子。实验结果显示,甲磺酸甲酯、甲磺酸乙酯、甲磺酸异丙酯对应色谱峰之间实现了基线分离,空白提取溶液无干扰;3种遗传毒性杂质在37~1 480 ng/mL范围内线性关系良好,且不同浓度水平平均回收率分别为104.99%、107.26%及108.85%,RSD均不超过4.54%。该方法具有专属、灵敏、准确、稳定、通用性好的特点,已用于多种不同来源市售甲磺酸中甲磺酸烷基酯类杂质的检测和控制。

     

    Abstract: An analytical liquid-liquid extraction-gas chromatography–mass spectrometry (LLE-GC-MS) method was established for the determination of genotoxic impurities including methyl methanesulfonate (MMS), ethyl methanesulfonate (EMS) and isopropyl methanesulfonate (IMS) in methanesulfonic acid. An Agilent HP-1MS capillary column (30 m × 0.32 m, 1 μm) was used for separating the analytes by programmed heating with the inlet temperature of 220 °C. Mass spectrometry was operated in positive ion mode, and selective ion monitors were set at m/z 80 for MMS, m/z 79 for EMS, m/z 123 for IMS and m/z 56 for internal standard butyl methanesulfonate (BMS). Results showed that the baseline separation of MMS, EMS and IMS was achieved, and the blank extraction solution had no interference; good linearity was achieved in the range of 37-1 480 ng/mL for three alkyl methanesulfonates; The mean recoveries of MMS, EMS, IMS were 104.99%, 107.26%,108.85%, respectively, with RSD ≤ 4.54%. The established method has the characteristics of good specific, sensitive, accurate, stable and versatility, and has been used for the detection and control of alkyl methanesulfonate impurities in methanesulfonic acid from a variety of manufacturers.

     

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