GC-MS法测定舒更葡糖钠中基因毒性杂质二甲氨基甲酰氯

GC-MS determination of genotoxic impurity dimethylcarbamoyl chloride in sugammadex sodium

目的 建立气相-质谱联用技术(GC-MS)测定舒更葡糖钠中基因毒性杂质二甲氨基甲酰氯。方法 毛细管柱为VF-624ms(30 m×0.25 mm,1.4μm),起始柱温为40℃,载气为氦气,柱流量为1.5 ml/min。质谱检测方式为选择离子模式(SIM),目标离子的m/z为107。结果 空白溶剂和舒更葡糖钠均不干扰二甲氨基甲酰氯的检测;二甲氨基甲酰氯的线性关系在8.08~80.80 ng/ml范围内表现良好(r=0.9999);平均回收率为100.91%(RSD=2.92%)(n=9);其检测限和定量限分别为4.04、8.08 ng/ml。结论 该测定方法专属性较好,简便、灵敏度高,能用于舒更葡糖钠中二甲氨基甲酰氯的检测。

Objective To establish a gas chromatography-mass spectrometry(GC-MS)for the determination of genotoxic impurity dimethylcarbamoyl chloride in sugammadex sodium.Methods The capillary column is VF-624 ms(30 m×0.25 mm,1.4μm),with an initial column temperature of 40℃,carrier gas of helium,and column flow rate of 1.5 ml/min.The mass spectrometry detection method is selected ion monitoring(SIM),and the m/z of the target ion is 107.Results The blank solvent and sugammadex sodium did not interfere with the detection of dimethylcarbamoyl chloride.The linear relationship of dimethylcarbamoyl chloride showed good performance in the range of 8.08-80.80 ng/ml(r=0.9999).The average recovery rate was 100.91%(RSD=2.92%)(n=9).The detection limit and quantification limit were 4.04 and 8.08 ng/ml,respectively.Conclusion This determination method has good specificity,simplicity,and high sensitivity,and it can be used for the detection of dimethylcarbamoyl chloride in sugammadex sodium.