高效液相色谱-质谱法测定注射用磺苄西林钠中D(-)型磺苄西林钠的含量

Determination of D(- ) Sulbenicillin Sodium in Sulbenicillin Sodium for Injection by HPLC-MS

目的 建立高效液相色谱串联质谱法测定注射用磺苄西林钠中D（-）型磺苄西林钠含量的方法。方法 采用SHIMADZu VP-ODS色谱柱进行分离,以0.01 mol·L-1乙酸铵溶液-甲醇（90∶10）为流动相,流速为0.6 mL·min-1。在ESI负离子模式下,采用多反应离子监测（MRM）扫描方式进行检测。结果 D（-）型及L（＋）型磺苄西林钠能够有效分离。D（-）型磺苄西林钠含量在1.03~51.90 μg·mL-1内与峰面积有良好的线性关系。在3个添加水平下,样品的加标回收率为99.98%,测定结果的相对标准偏差为0.30%（n=9）。结论 MRM方法定量准确、可靠,可用于注射用磺苄西林钠中D（-）型磺苄西林钠的含量检测。

To establish a method for determination of D（-） sulbenicillin sodium in sulbenicillin sodium for injection by HPLC/MS. METHODS The analysis was performed on a SHIMADZU VP-ODS column with mobile phase consisting of 0.01 mol·L-1 ammonium acetate solution-methanol （90∶10） at a flow rate of 0.6 mL·min-1. The detection was performed by Multiple Reaction Monitoring （MRM） scanning mode with ESI negative ion mode. RESULTS D（-） and L（＋） sulbenicillin could be effectively separated. Good liner relationship was achieved when the concentration of D（-） sulbenicillin was in the range of 1.03-51.90 μg·mL-1（r=0.999 7）. The average recovery rate was 99.98% at three levels （RSD=0.30%, n=9）. CONCLUSION The MRM method is accurate, reliable, and can be used for the determination of D（-） sulbenicillin sodium in sulbenicillin sodium for injection.