高效液相色谱法测定头孢曲松钠中2-巯基苯并噻唑含量

摘要：目的 建立测定头孢曲松钠中基因毒性杂质2-巯基苯并噻唑含量的反相高效液相色谱法。方法 采用十八烷基硅烷键合硅胶为填充剂(Agilent ZORBAX SB-Aq C18，4.6 mm×250 mm，5 μm)的色谱柱，流动相为1%甲酸溶液-乙腈(60:40，V/V)，流速0.5 mL/min，检测波长320 nm，柱温25℃。结果 定量限为0.5 ppm(相当于样品浓度的百分比为0.00005%)，检测限为0.15 ppm。2-巯基苯并噻唑在0.0051~0.2051 μg/mL浓度范围内，线性方程为y=6.4195x-0.0098，r=0.9996＞0.999。回收率为86.3%~102.3%(RSD＜10.0%，n=9)。结论 该方法操作简便、专属性强、灵敏度高，可有效检出头孢曲松钠中2-巯基苯并噻唑的含量。

Determination of 2-mercaptobenzothiazole in ceftriaxone sodium by HPLC

Abstract Objective To establish an RP-HPLC method for the determination of 2-mercaptobenzothiazole inceftriaxone sodium. Methods Agilent Zorbax SB-AQ C18 (4.6 mm×250 mm, 5 μm) was used. The mobile phase waswater containing 1% formic acid-acetonitrile (60:40, V/V). The flow rate was 0.5 mL/min. The detection wavelengthwas 320 nm and the column temperature was 25℃. Results The LOQ was 0.5 ppm (corresponding to a percentageof sample concentration 0.00005%) and the LOD was 0.15 ppm. The caliblation curve for 2-mercurbenzothiazolewas linear in the concentration range of 0.0051 μg/mL to 0.2051μg/mL (y=6.4195x-0.0098，r=0.9996＞0.999). Therecoveries were 86.3% to 102.3% (RSD<10.0%, n=9). Conclusion The method is simple, specific, and sensitive forthe determination of 2-mercaptobenzothiazole in ceftriaxone