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    LC-MS测定醋酸甲羟孕酮中对甲苯磺酸甲酯及对甲苯磺酸乙酯的含量

    Determination of Methyl p-Toluenesulfonate and Ethyl p-Toluenesulfonate in Medroxyprogesterone Acetate by LC-MS

      摘要
    • 摘要: 目的 建立醋酸甲羟孕酮中的基因毒性杂质对甲苯磺酸甲酯及对甲苯磺酸乙酯的LC-MS检测方法。方法 采用XDB-C18（50 mm×4.6 mm，1.8 μm）色谱柱；10 mmol·L-1醋酸铵（氨水pH 7.0）-乙腈为流动相；质谱：正离子模式，检测离子m/z 187.1，201.1。结果 对甲苯磺酸甲酯和对甲苯磺酸乙酯在0.05~5.08 μg·mL-1内线性关系良好。对甲苯磺酸甲酯定量限为0.1 ng，检测限均为0.05 ng；对甲苯磺酸乙酯定量限为0.03 ng，检测限为0.02 ng；对甲基苯磺酸甲酯平均回收率101.6%，RSD为3.46%；对甲基苯磺酸乙酯平均回收率98.7%，RSD为2.22%。结论 本方法适用于样品醋酸甲羟孕酮中对甲基苯磺酸甲酯和对甲基苯磺酸乙酯的检测。

       

      Abstract: OBJECTIVE To establish a method for detecting genotoxin methyl p-toluenesulfonate and ethyl p-toluenesulfonate in medroxyprogesterone acetate by LC-MS.METHODS The determination was peformed on XDB-C18 column (50 mm×4.6 mm, 1.8 μm) with mobile phase A(10 mmol·L-1 ammonium acetate, adjust pH to 7.0 with aqueous ammonia) and mobile phase B(acetonitrile). The mass spectrometer was performed in SIM m/z:187.1, 201.1 by positive monitoring.RESULTS Both of methyl p-toluenesulfonate and ethyl p-toluenesulfonate were linear in the range of 0.05-5.08 μg·mL-1. LOQ and LOD of methyl p-toluenesulfonate was 0.10 ng and 0.05 ng, LOQ and LOD of ethyl p-toluenesulfonate was 0.03 ng and 0.02 ng. Their recoveries were 101.6% and 98.7%, with RSDs of 3.46% and 2.22%, respectively.CONCLUSION This method is applicable to the detection of methyl p-toluenesulfonate and ethyl p-toluenesulfonate in medroxyprogesterone acetate.

       

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