气相色谱-质谱法测定氟维司群注射液中的氯化苄和二氯化苄
Determination of Benzyl Chloride and Benzyl Dichloride in Fulvestrant Injection by GC-MS
郑华 1卢红华 1何艳琴 1郝贵周 1张贵民1
作者信息
- 1. 鲁南制药集团股份有限公司,国家手性制药工程技术研究中心,山东临沂 273400
- 折叠
摘要
建立了气相色谱-质谱(GC-MS)法测定氟维司群注射液(1)中的遗传毒性杂质氯化苄(2)、二氯化苄(3).采用VF-lms毛细管柱(0.25 mm×30 m×0.25μm),采用2种监测模式,分别对2(MRM)与3(SIM)进行测定.结果显示,2和3分别在5.427～54.272、4.775～47.748 ng/mL内线性关系良好,定量限分别为2.714、2.387 ng/mL,检测限分别为0.54、0.48 ng/mL,平均回收率(n=9)分别为99.43％、99.09％,RSD分别为2.43％、2.66％.建立的GC-MS法可为1中的杂质研究提供参考.
Abstract
A gas chromatography-mass spectrometry(GC-MS)method was established to determine the genotoxic impurities of benzyl chloride(2)and benzyl dichloride(3)in fulvestrant injection(1).The VF-lms capillary column(0.25 mm×30 m×0.25 μm)was used,and two monitoring modes were respectively adopted to measure 2(MRM)and 3(SIM).The results showed that it was linear for 2 and 3 in the ranges of 5.427-54.272 ng/mL,4.775-47.748 ng/mL,respectively.The LOQs of 2 and 3 were 2.714 and 2.387 ng/mL,and the LODs were 0.54 and 0.48 ng/mL,respectively.The average recoveries(n=9)of 2 and 3 were 99.43％and 99.09％,with the RSDs of 2.43％and 2.66％,respectively.The established GC-MS method can provide references for impurity research in 1.
关键词
气相色谱-质谱/氟维司群注射液/氯化苄/二氯化苄Key words
GC-MS/fulvestrant injection/benzyl chloride/benzyl dichloride引用本文复制引用
出版年
2024
NETL
NSTL
万方数据