衍生化GC-MS法测定甲磺酸萘莫司他原料药中甲磺酸甲酯与甲磺酸乙酯

Determination of mthylmesylate and ethylmesylate in nafamostat mesilate raw material by derivative GC-MS

目的建立衍生化GC-MS法测定甲磺酸萘莫司他原料药中甲磺酸甲酯与甲磺酸乙酯。方法采用柱前衍生技术、程序升温法,以氦气为载气,以甲磺酸丁酯为内标,测定甲磺酸萘莫司他中甲磺酸甲酯和甲磺酸乙酯的含量。结果甲磺酸甲酯和甲磺酸乙酯的线性范围均为3.0~200.0ng·mL^(-1),相关系数分别为0.997 5和0.999 9;检测限分别为0.964 3和1.007 8ng·mL^(-1);定量限分别为2.892 8和3.022 3ng·mL^(-1);进样精密度的RSD值分别为0.9%和1.3%;平均加样回收率分别为102%(RSD=2.9%)和106%(RSD=1.2%)。结论该方法简单方便、快速易行,可作为控制甲磺酸萘莫司他中甲磺酸甲酯与甲磺酸乙酯含量的有效方法。

To determinate mthylmesylate(MMS)and ethylmesylate(EMS)in nafamostat mesilate raw material by derivative GC-MS.The MMS and EMS were determined by pre-column derivation by temperature programming method.Helium was used as the carrier gas.The content of MMS and EMS were quantified with butylmesylate as internal standard.The linear calibration curves of MMS and EMS were both obtained over the range of 3.0-200.0 ng.mL 1,the correlation coefficients were 0.997 5 and 0.999 9.The limits of detection were 0.964 3 and 1.007 8 ng.mL 1,the limits of quantitation were 2.892 8 and 3.022 3 ng.mL The RSDs of the injection precision were 0.9%and 1.3%.The extraction rates were 102%and 106%with RSD of 2.9%and 1.2%.The method is simple and convenient,quick and easy,and can be used for the quality control of MMS and EMS in nafamostat mesilate.