HPLC法测定原料药AL58805中基因毒杂质  

Determination of Genotoxic Impurities in AL58805 by HPLC

作　　者：朱小华 吕列超 赵金亮 刘巧云[2] 夏玥 张迪 Zhu Xiaohua;Lv Liechao;Zhao Jinliang;Liu Qiaoyun;Xia Yue;Zhang Di(Changzhou Jiade Pharmtech Co.,Ltd.,Jiangsu Changzhou 213164,China;Changzhou Institute of Engineering Technology,Jiangsu Changzhou 213164)

机构地区：[1]常州佳德医药科技有限公司,江苏常州213164 [2]常州工程职业技术学院,江苏常州213164

出　　处：《化工时刊》2020年第2期17-20,共4页Chemical Industry Times

摘　　要：目的建立一种高效液相色谱法测定AL58805原料药中基因毒性杂质对甲苯磺酸甲酯、对甲苯磺酸乙酯的方法。方法采用InertSustain C18色谱柱(4.6×250 mm,5μm);以0.015 mol·L-1磷酸水溶液-乙腈(50∶50,V/V)为流动相;检测波长为225 nm;流速为1 mL·min-1。结果对甲苯磺酸甲酯在3.320~200 ng·mL-1、对甲苯磺酸乙酯在4.550~200 ng·mL-1的范围内浓度与峰面积呈良好的线性关系(R 2=0.9997、R 2=0.9992);检测限分别为3.320 ng·mL-1、4.550 ng·mL-1;定量限分别为9.960 ng·mL-1、13.64 ng·mL-1;平均回收率分别为92.06%、101.4%,RSD均为2.8%(n=9)。结论本法简单快捷、灵敏度高,可用于AL58805原料药中基因毒杂质对甲苯磺酸甲酯、对甲苯磺酸乙酯的检测。Objective:To establish a high performance liquid chromatography method for the determination of genotoxic impurities such as methyl p-toluenesulfonate and ethyl p-toluenesulfonate in AL58805 bulk drug.Methods InertSustain C18 column(4.6×250 mm,5μm)was used;the mobile phase was 0.015 mol·L-1 phosphoric acid aqueous solution-acetonitrile(50∶50,V/V);the detection wavelength was 225 nm;the flow rate was 1 mL·min-1.Results:The concentration of methyl p-toluenesulfonate in the range of 3.320~200 ng·mL-1 and ethyl p-toluenesulfonate in the range of 4.550~200ng·mL-1 showed a good linear relationship with the peak area(R 2=0.9997,R 2=0.9992).The detection limits are 3.320 ng·mL-1 and 4.550 ng·mL-1,respectively.The quantification limits were 9.960 ng·mL-1 and 13.64 ng·mL-1,respectively;the average recoveries were 92.06%and 101.4%,respectively,and the RSD was 2.8%(n=9).Conclusion:This method is simple,rapid and sensitive.It can be used for the detection of methyl p-toluenesulfonate and ethyl p-toluenesulfonate in AL58805.

关 键 词：高效液相色谱法 AL58805 基因毒杂质 对甲苯磺酸甲酯 对甲苯磺酸乙酯 

分 类 号：O657.72[理学—分析化学] TQ460.72[理学—化学]