摘要
目的建立气相色谱-质谱联用法,测定拉洛他赛原料中基因毒杂质三氟甲磺酸乙酯。方法采用6%氰丙基苯基和94%二甲基聚硅氧烷为固定相的毛细管柱(DB-624,30 m×0.25 mm×1.4μm),EI源,以起始温度为50℃,维持6 min,以30℃/min的速率升温至230℃,250℃下运行3 min;流速为1.0 mL·min^(-1)。结果三氟甲磺酸乙酯检测限为1.81ppb,定量限为6.15ppb,三氟甲磺酸乙酯在3.65~584.62 ng·mL^(-1)浓度范围内线性关系良好(r=0.9998),方法回收率(n=9)均在95.4%~111.4%范围内,RSD<5.6%。结论方法简便、准确,灵敏度高,专属性强,可用于拉洛他赛原料中三氟甲磺酸乙酯基因毒杂质的测定。
OBJECTIVE To establish a gas chromatography-mass spectrometry method for the determination of ethyl trifluoromethanesulfonate,a genotoxic impurity,in raw materials of lalotaxel.METHODS A capillary column(DB-624,30 m×0.25 mm×1.4μm)with 6%cyanopropylphenyl and 94%dimethylpolysiloxane as the stationary phase was used,the EI source was used,and the initial temperature was 50℃,maintained for 6 minutes,heated to 230℃at a rate of 30℃per minute,and operated at 250℃for 3 minutes;the flow rate was 1.0 mL·min^(-1).RESULTS The detection limit of ethyl trifluoromethanesulfonate was 1.81ppb,and the limit of quantification was 6.15ppb.The linear relationship of ethyl trifluoromethanesulfonate in the concentration range of 3.65-584.62 ng·mL^(-1)was good(r=0.9998),and the method was recovered.The rate of quantification(n=9)was in the range of 95.4%-111.4%,the RSD was less than 5.6%.CONCLUSION The method is simple,accurate,sensitive and specific,and can be used for the determination of ethyl trifluoromethanesulfonate genotoxic impurities in larotaxel raw materials.
作者
王潞娜
王红芳
张志成
柴青叶
宋小飞
张辉
WANG Lu-na;WANG Hong-fang;ZHANG Zhi-cheng;CHAI Qing-ye;SONG Xiao-fei;ZHANG Hui(Shanxi Zhendong Pharmaceutical Co.,Ltd.,Changzhi 047100,China)
出处
《海峡药学》
2023年第1期60-63,共4页
Strait Pharmaceutical Journal