HPLC法测定注射用盐酸头孢吡肟中2-巯基苯并噻唑

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，5 μm)，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10 μL。结果 2-巯基苯并噻唑在浓度 0.01~102.9 μg/mL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。

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

Abstract 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 elutionwas 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/mL~102.9 μg/mL (r=0.9999) for 2-mercaptobenzothiazole. The regression equation is y=70652x+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