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

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, 3.2 μm)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1.5804~2.6340 μg/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。

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

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．