高效液相色谱-质谱法测定伏格列波糖片中伏格列波糖含量

Quantitative determination of voglibose contents in its tablets with high-performance liquid chromatography-mass spectrometry

目的：建立高效液相色谱-质谱法测定伏格列波糖片中伏格列波糖的含量。方法：采用Agilent ZORBAX Eclipse Plus C18（2．1 mm ×150 mm，3．2μm）色谱柱，柱温40℃，流速为0．25 ml/min，甲醇-水（2∶3）为流动相，流速为0．25 ml/min，质谱检测中采用电喷雾离子源多反应检测扫描（ MRM）模式。结果：伏格列波糖浓度在1．5804～2．6340μg/ml范围内线性关系良好，其中离子对268．2/74．2（r＝0．9990）平均回收率为100．2％，相对标准偏差为1．37％（ n＝6）；离子对268．2/92．2（r＝0．9976）平均回收率为99．3％，相对标准偏差为1．78％（n＝6）。结论：高效液相色谱-质谱法准确性、重复性均好，可用于伏格列波糖片的质量控制。

Objective：To develop a method for determination of voglibose contents in its tablets by high-performance liquid chromatography-mass spectrometry （ HPLC-MS） .Methods：The measurements were carried out on an Agilent ZORBAX Eclipse Plus C18 column （2.1 ×150mm 3.2μm） with a temperature of 40℃.A mixture of methanol and water （2∶3, v/v） was used as a mobile phase at a flow rate of 0.25 ml/min.Voglibose was detected in an electrospray ionization （ESI） mode with MRM. Results：The calibration curves of voglibose showed good linearity in a range of 1 .5804-2.6340 μg/ml （r=0.9990）.The average recovery was 100.2%with RSD of 1.37%（ n=6 ） for m/z 268 .2/74 .2 .Linearity was obtained with r=0 .9976 and the average recovery was 99.3%with RSD of 1.78%（n=6） for m/z 268.2/92.2.Conclusion：HPLC-MS method is accurate , reproducible and can be used for quality control of voglibose tablets .