目的 采用高效液相色谱-串联质谱技术（HPLC-MS/MS），建立同时测定某“中药保健品”中非法添加的4种降糖药二甲双胍、苯乙双胍、罗格列酮、格列苯脲的方法。方法 采用Thermo BDS Hypersil C8（2.1 mm × 100 mm，2.4 μm）色谱柱，0.2 %甲酸水溶液（A）和乙腈-甲醇（6∶4，v/v）（B）为流动相进行梯度洗脱，流速0.3 mL·min-1，在电喷雾正离子模式下，以多反应监测（MRM）模式测定，定量离子对为m/z 129.9 → 70.9（二甲双胍）、m/z 205.9→59.9（苯乙双胍）、m/z 357.9→134.9（罗格列酮）、m/z 494.0→169.0（格列苯脲）。结果 同时检出了4种降血糖化学药物。检出限为0.06～0.5 ng·mL-1，定量限为0.21～1.62 ng·mL-1，在3个不同浓度的添加水平下，4种化学药物的平均回收率为66.3 %～110.2 %，相对标准偏差（RSD）为2.3 %～12.2 %。结论 该方法可快速、准确地检测保健食品中非法添加二甲双胍、苯乙双胍、罗格列酮、格列苯脲4种降血糖化学药，具有专属性强、灵敏度高的特点。

Objective To develop a HPLC-MS/MS method for simultaneous quantification of metformin，phenformin，rosiglitazone，and glibenclamide，four antidiabetics which were illegally added into a health-care food. Methods The separation was performed on a Thermo BDS Hypersil C8 column（2.1 mm×100 mm，2.4 μm） by gradient elution with the mixture of 0.2 % aqueous formic acid（A） and acetonitrile-methanol（6∶4，v/v）（B） as mobile phase. The flow rate was set at 0.3 mL·min-1. The detection of 4 target chemicals was performed by positive-ion electrospray ionization mass spectrometry（ESI-MS） in multiple-reaction monitoring（MRM） mode. The transitions of four antidiabetics executed as following：m/z 129.9→70.9 for metformin，m/z 205.9→ 9.9 for phenformin，m/z 357.9→134.9 for rosiglitazone，m/z 494.0→368.8 for glibenclamide. Results Four antidiabetics had been simultaneously identified from the health-care food by the established method. The limits of detection（LOD，S/N≥3） and quantitation（LOQ，S/N≥10）were 0.06~0.5 ng·mL-1 and 0.21~1.62 ng·mL-1，respectively. The average recoveries of the four analytes at three spiked concentration levels were 66.3 % to 110.2 % with relative standard deviations（RSDs） at 2.3 %~12.2 %. Conclusion The established method is convenient，rapid and accurate，and can be used for simultaneous determination of multiple antidiabetics in a health-care food which is labeled as a product of pure medicinal herbs.

R284.1