LC-MS法测定新型VMAT2抑制剂LPM3770164中的樟脑磺酸酯

Determination of Camphor Sulfonate in New VMAT2 Inhibitor LPM3770164 by LC-MS

本文建立了LC-MS法对LPM3770164中的樟脑磺酸甲酯(MCS)、樟脑磺酸乙酯(ECS)进行定量检测。采用色谱柱ACQUITY UPLC Peptide CSH C18(150 mm×2.1 mm,1.7μm),以10 mmol·L^(-1)乙酸铵溶液-乙腈(90∶10,V/V)为流动相A、乙腈为流动相B进行梯度洗脱。质谱采用电喷雾正离子化选择离子监测模式进行检测。经方法学验证结果表明,MCS在1.97~14.79 ng·mL^(-1)内线性关系良好(r=0.9999);ECS在1.90~14.26 ng·mL^(-1)内线性关系良好(r=0.9999)。通过加样回收率试验,MCS、ECS的平均回收率(n=9)分别为98.5%、99.1%。研究表明该方法操作简便,灵敏度高,可用于LPM3770164中樟脑磺酸甲酯、樟脑磺酸乙酯的测定,并为其质量控制提供参考。

An LC-MS method is established for the quantitative determination of methyl camphor sulfonate(MCS)and ethyl camphor sulfonate(ECS)in LPM3770164.The separation is achieved on ACQUITY UPLC Peptide CSH C18(150 mm×2.1 mm,1.7μm)using 10 mmol·L^(-1)ammonium acetate solution-acetonitrile(90∶10,V/V)as mobile A and acetonitrile as mobile phase B in gradient elution mode.The positive ion electrospray ionization method and SIM scanning mode are used in MS to detect the genotoxic impurities of camphor sulfonate.Methodological verification results show that MCS has a good linear relationship between 1.97 and 14.79 ng·mL^(-1)(r=0.9999),and ECS has a good linear relationship between 1.90 and 14.26 ng·mL^(-1)(r=0.9999).The average recoveries of MCS and ECS are 98.5%and 99.1%(n=9),respectively.The method is simple and sensitive,and can be used to determine methyl camphor sulfonate and ethyl camphor sulfonate in LPM3770164,and provide reference for its quality control.