高效液相色谱法测定盐酸布替萘芬中两种基因毒性杂质  

Determination of Genotoxic Impurities 1-Chloromethyl Naphthalene and 4-tert-Butylbenzyl Chloride in Butenafine Hydrochloride by High Performance Liquid Chromatography

作　　者：戚安金 刘发贵 徐志贫 刘思光 李铁健 张贵民 QI An-jin;LIU Fa-gui;XU Zhi-pin;LIU Si-guang;LI Tie-jian;ZHANG Gui-min(Shandong New Time Pharmaceutical Co,Ltd,Linyi 273400,China;Lunan Pharmaceutical Group Co,Ltd,Linyi 276002,China)

机构地区：[1]山东新时代药业有限公司,山东临沂273400 [2]鲁南制药集团股份有限公司,山东临沂276002

出　　处：《海峡药学》2022年第3期97-99,共3页Strait Pharmaceutical Journal

摘　　要：目的 建立高效液相色谱法测定盐酸布替萘芬中两种基因毒性杂质1-氯甲基萘和对叔丁基苄氯的残留。方法 色谱柱YMC Triart C_(18)(4.6×250 mm,3μm),流动相0.1%磷酸水溶液∶乙腈=45∶55,流速1.0 mL·min^(-1),紫外检测波长220 nm。结果 1-氯甲基萘、对叔丁基苄氯保留时间、分离度良好,空白无干扰。一定浓度范围内,1-氯甲基萘、对叔丁基苄氯线性关系良好,r分别为0.9998、0.9997。1-氯甲基萘的加标回收率(n=9)范围为90.21%~94.69%,RSD为1.4%;对叔丁基苄氯的加标回收率(n=9)范围为89.13%~93.59%,RSD为1.7%。结论 本法操作简便,测定结果准确,重复性好,可用于盐酸布替萘芬中两种基因毒性杂质1-氯甲基萘和对叔丁基苄氯的检测,为药品质量的控制提供了重要参考依据。OBJECTIVE To establish a High Performance Liquid Chromatography(HPLC) method for determination of two genotoxic impurities 1-chloromethylnaphthalene and 4-tert-butylbenzyl chloride in butenafine hydrochloride.METHODS The separation was performed on a YMC Triart C_(18) column(4.6×250 mm,3 μm) by linear elution using 0.1% phosphoric acid buffer solution-acetonitrile(gradient elution),the flow rate was 1.0 mL·min^(-1) and the UV detection wavelength was 220 nm.RESULTS The retention time and resolution of 1-chloromethylnaphthalene and 4-tert-butylbenzyl chloride were affable,and the blank was non-interfering.Within a certain concentration range,the linear relationship of 1-chloromethylnaphthalene and 4-tert-butylbenzyl chloride was good,and the r were 0.9998 and 0.9997 respectively.The standard recovery rate of 1-chloromethyl naphthalene(n=9) ranged from 90.21% to 94.69%,and the RSD was 1.4%;The standard recovery rate of 4-tert-butylbenzyl chloride(n=9) ranged from 89.13% to 93.59%,and the RSD was 1.7%.CONCLUSION The method is easy to operate,accurate and reproducible,which can be used for the detection of 1-chloromethylnaphthalene and 4-tert-butylbenzyl chloride in butenafine hydrochloride.It provides an important reference for drug quality control.

关 键 词：盐酸布替萘芬 基因毒性杂质 1-氯甲基萘 对叔丁基苄氯 

分 类 号：R927[医药卫生—药学]