Ranbaxy Research Laboratory, Sector 18, Plot No. 20, Udyog Vihar Industrial Area, Gurgaon 122015, Haryana, India.
J Pharm Biomed Anal. 2011 May 15;55(2):379-84. doi: 10.1016/j.jpba.2011.01.039. Epub 2011 Feb 24.
Methyl methanesulfonate (MMS) and ethyl methanesulfonate (EMS) have been highlighted as potential genotoxic impurities (PGIs). A sensitive LC/MS/MS method is developed and validated for the determination of MMS and EMS impurities in both Lopinavir and Ritonavir Active pharmaceutical ingredient. Method utilizes, Atlantis T3 column with electrospray ionization in multiple reactions monitoring (MRM) mode for quantitation of impurities. The proposed method is specific, linear, accurate and precise. The calibration curves show good linearity over the concentration range of 0.01-0.23 μg/mL for MMS and 0.005-0.23 μg/mL for EMS. The correlation coefficient obtained is >0.99 in each case. Method has very low limit of detection (LOD) and quantification (LOQ). LOD and LOQ of MMS and EMS are as low as ∼0.002 μg/mL and ∼0.01 μg/mL respectively. Method has accuracy within 80-120% for both the analytes. This method is a good quality control tool for quantitation of MMS and EMS impurities at very low levels in Lopinavir and Ritonavir.
甲磺酸甲酯（MMS）和乙磺酸乙酯（EMS）已被确定为潜在的遗传毒性杂质（PGI）。本研究开发并验证了一种灵敏的 LC/MS/MS 方法，用于测定洛匹那韦和利托那韦原料药中的 MMS 和 EMS 杂质。该方法采用 Atlantis T3 柱，以电喷雾电离多反应监测（MRM）模式进行定量分析。所提出的方法具有特异性、线性、准确性和精密度。校准曲线显示 MMS 的浓度范围为 0.01-0.23μg/mL，EMS 的浓度范围为 0.005-0.23μg/mL，均具有良好的线性关系。每种情况下的相关系数均大于 0.99。该方法的检测限（LOD）和定量限（LOQ）非常低。MMS 和 EMS 的 LOD 和 LOQ 分别低至约 0.002μg/mL 和约 0.01μg/mL。该方法对两种分析物的准确度在 80-120%之间。该方法是一种很好的质量控制工具，可用于定量测定洛匹那韦和利托那韦中非常低水平的 MMS 和 EMS 杂质。
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