HPLC法测定注射用盐酸头孢吡肟中2-巯基苯并噻唑  

Determination of 2-mercaptobenzothiazole in cefepime hydrochloride for injection by HPLC

作　　者：肖慧[1] 王婷婷[1] 吴文获 洪建文[1] Xiao Hui;Wang Ting-ting;Wu Wen-huo;and Hong Jian-wen(Guangdong Institute for Food and Drug Control,NMPA Key Laboratory for Rapid Testing Technology of Drugs,Guangzhou 510180;Dongguan Qingxi Town Community Health Service,Dongguan 523660)

机构地区：[1]广东省药品检验所,国家药品监督管理局药品快速检验技术重点实验室,广州510180 [2]东莞市清溪镇社区卫生服务中心,东莞523660

出　　处：《中国抗生素杂志》2022年第2期183-188,共6页Chinese Journal of Antibiotics

基　　金：广东省省级科技计划项目(No.2018B020207008)。

摘　　要：目的 建立HPLC法测定注射用盐酸头孢吡肟中2-巯基苯并噻唑基因毒性杂质含量的方法。方法 HPLC法,采用Inertsil ODS-3柱(250 mm×4.6 mm,5μm),以50 mmol/L磷酸氢二钠溶液(用磷酸调pH值至6.25)-甲醇-80%乙腈(60:10:30,V/V/V)为流动相,等度洗脱,流速为1 mL/min,柱温为35℃,检测波长为320 nm,进样体积为10μL。结果 2-巯基苯并噻唑在浓度0.01~102.9μg/m L范围内,呈良好的线性关系,回归方程y=70652x+2167.2,相关系数r=0.9999;定量限为0.3 ng,检测限为0.1 ng,回收率均值(n=9)为91.7%。结论 本方法专属性强、准确、快捷、灵敏且耐用性良好,为测定注射用盐酸头孢吡肟中2-巯基苯并噻唑含量的有效补充检测与定量方法,并为该产品临床应用安全性提供保障。Objective To establish of an HPLC method for determination of 2-mercaptobenzothiazole genotoxic impurities in cefepime hydrochloride for injection. Methods The HPLC analysis was performed on a Inertsil ODS-3 column(250 mm×4.6 mm, 5 μm) with a mobile phase of 50 mmol/L disodium hydrogen phosphate solution(adjust pH value of phosphoric acid to 6.25)-methanol-80% acetonitrile(60:10:30, V/V/V). Isocratic elution was used. The flow rate was 1.0 mL/min. The detection wavelength was 320 nm and the column temperature was 35□,and the injection volumn was 10 μL. Results The calibration curve was linear within the range of 0.01 μg/m L~102.9 μg/m L(r=0.9999) for 2-mercaptobenzothiazole. The regression equation is y=70652 x+2167.2. The limit of quantitation was 0.3 ng. The detection limit was 0.1 ng. The recoveries(n=9) were 91.7%. Conclusion This method has strong specificity,accuracy, rapidity, sensitivity, and good durability. It is an effective supplementary detection and quantitative method for the determination of 2-mercaptobenzothiazole in cefepime hydrochloride for injection, and provides guarantee for the safety of clinical application of the product.

关 键 词：注射用盐酸头孢吡肟 2-巯基苯并噻唑 基因毒性杂质 含量 HPLC法 

分 类 号：R978.1[医药卫生—药品] R917[医药卫生—药学]