高效液相色谱-串联质谱法测定艾瑞昔布片中艾瑞昔布的含量

CONTENT DETERMINATION OF IMRECOXIB IN IMRECOXIB TABLETS BY LC-MS/MS

目的 建立测定艾瑞昔布片剂中艾瑞昔布的高效液相色谱-串联质谱（liquid chromatography-mass sepectrometry,LC-MS/MS）含量测定方法.方法 样品经甲醇-水（80∶20,V/V）提取,0.22μm微孔滤膜滤过后采用LC-MS/MS法测定其中艾瑞昔布的含量.色谱柱为Waters Symmetry R C18（3.5μm,2.1mm×100mm）,流动相为乙腈-水,梯度洗脱;离子源为电喷雾离子化源（ESI源）,离子源温度为550 ℃,以多反应监测方式分别监测离子对m/z 370.2~278.2（艾瑞昔布）和m/z 346.1~198.0（内标奥美拉唑）.结果 艾瑞昔布的监测浓度在31.83~509.34μg/L范围内与内标的峰面积比值呈良好线性关系（r=0.997 6）;平均加样回收率在95.6%~103.4%范围内,相对标准差均小于6.1%（n=9）.结论该方法快速、灵敏,结果准确,适用于艾瑞昔布片剂的质量控制.

Objective To establish a high performance liquid chromatography-mass sepectrometry （LC-MS/MS） method for the determination of imrecoxib in imrecoxib tablets.Methods The samples were firstly extracted with film.The content of imrecoxib was determined by LC-MS/MS.The determination was performed on Waters Symmetry R C18 （3.5μm,2.1mm×100mm） column with gradient elution.The mass spectrometer was operated in the positive ionization electrospray（ESI） mode using multiple reaction monitoring for analysis of imrecoxib at 550℃.The transitions of m/z 370.2-278.2（imrecoxib） and m/z 346.1-198.0 （omeprazole） were used to quantify imrecoxib and omeprazole.Results The linear range of imrecoxib was 31.83-509.34μg/L（r=0.997 6） and the method recovery was within 95.6%-103.4% （RSD＜6.1%,n=9）.Conclusion The method is rapid,sensitive and accurate,and it is suitable for the quality control of imrecoxib tablets.