HPLC测定4-邻甲苯磺酰氧基苯并噁唑酮原料药的含量及有关物质

Determination of Crude Drug 4-O-Methyl-benzenesulfonyl-2(3H)-benzoxazolone and Its Related Substances by HPLC

关键词:  4-邻甲苯磺酰氧基苯并噁唑酮  含量测定  有关物质  高效液相色谱法

Key words:  4-O-methyl-benzenesulfonyl-2(3H)-benzoxazolone  content determination  related substances  HPLC

摘要:

目的 建立高效液相色谱法测定非甾体抗炎镇痛化合物4-邻甲苯磺酰氧基苯并噁唑酮(MBB)原料药的含量及有关物质。方法 采用Odyssil C₁₈(150 mm×4.6 mm，5 μm)色谱柱，以甲醇-水(65∶35)为流动相，流速为0.8 mL·min^?1，检测波长为273 nm，柱温为25℃。结果 供试品中主成分峰与各杂质峰分离良好，MBB的线性范围为1~150 μg·mL^?1，回归方程为A=3 959.8C-2 831(r=0.999 7)，平均回收率为99.2%(RSD=1.1%，n=9)，检测限为1 ng。结论 本方法简便、准确、专属性好，可用于MBB原料药的含量测定及有关物质检查。

Abstract:

OBJECTIVE To establish an HPLC method for determining the content of non-steroidal anti-inflammatory compound 4-O-methyl-benzenesulfonyl-2(3H)-benzoxazolone(MBB) and its related substances. METHODS The chromato- graphic separation was performed on an Odyssil C₁₈ column (150 mm×4.6 mm, 5 μm). The mobile phase was consisted of methanol-water(65∶35) at a flow rate of 0.8 mL·min^?1. The detection wavelength was set at 273 nm and the column temperature was 25 ℃. RESULTS MBB was completely separated from impurities. The linear range was 1-150 μg·mL^?1, and the regression equation was A=3 959.8C-283 1(r=0.999 7). The average recovery was 99.2%(RSD=1.1%, n=9). The limit of detection was 1 ng. CONCLUSION The analytical method was simple, accurate and selective for the analysis of crude drug MBB and its related substances.