HPLC法测定来曲唑中苄基氯类基因毒性杂质  

Determination of the Genotoxic Benzyl Chlorides in Letrozole by HPLC

作　　者：潘再秀 常天歌 朱建 赵冬梅 曹志凌 PAN Zaixiu;CHANG Tiange;ZHU Jian;ZHAO Dongmei;CAO Zhiling(Jiangsu Ocean University,Lianyungang 222005;Lianyungang Guike Pharmaceutical Co.,Ltd.,Lianyungang 222000)

机构地区：[1]江苏海洋大学,江苏连云港222005 [2]连云港贵科药业有限公司,江苏连云港222000

出　　处：《中国医药工业杂志》2022年第9期1318-1321,共4页Chinese Journal of Pharmaceuticals

基　　金：江苏省产学研合作项目(BY2020579);江苏省研究生科研与实践创新项目(SJCX20-1232,SJCX20-1220,SJCX20-1225)。

摘　　要：建立了HPLC法测定来曲唑(1)原料药中苄基氯类基因毒性杂质对氰基二氯苄(2)和4-(1H-1,2,4-三唑-1-基氯甲基)苯甲腈(3)。色谱柱采用Alltima C_(18)柱(4.6 mm×250 mm,5μm),流动相A为水,B为乙腈,梯度洗脱,检测波长为230 nm,柱温为25℃,流速为1.0 ml/min。结果显示,2和3分别在0.0148~0.9337μg/ml、0.0286~0.8715μg/ml内线性良好,平均回收率(n=9)分别为99.9%和98.9%,RSD分别为0.59%和0.52%。建立的方法准确性好、灵敏度高,适用于1原料药中苄基氯类基因毒性杂质的检测。An HPLC method was established for the determination of the genotoxic impurities:p-cyano-benzyl dichloride(2)and 4-[chloro(1H-1,2,4-triazol-1-yl)methyl]benzonitrile(3)in letrozole(1).The Alltima C_(18) column(4.6 mm×250 mm,5μm)was used,and the analysis was carried out in the gradient elution mode with water as mobile phase A,and acetonitrile as mobile phase B.The detection wavelength was 230 nm,the column temperature was 25℃,and the flow rate was 1.0 ml/min.The results showed that it was linear for 2 and 3 in the ranges of 0.0148-0.9337μg/ml and 0.0286-0.8715μg/ml,respectively.And the average recoveries(n=9)of 2 and 3 were 99.9%and 98.9%,with the RSDs of 0.59%and 0.52%.The established method has good accuracy and high sensitivity,which is suitable for the detection of the genotoxic benzyl chlorides in 1.

关 键 词：高效液相色谱 来曲唑 基因毒性杂质 对氰基二氯苄 4-(1H-1 2 4-三唑-1-基氯甲基)苯甲腈 

分 类 号：R917[医药卫生—药物分析学]