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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(2.1mm×100 mm,2.4滋m)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 establish a method for the simultaneous determination of four antidiabetic drugs metformin, phenformin and rosiglitazone, which are illegally added in some “Chinese herbal health products” by HPLC-MS / MS. Method for the determination of phenylurea. Methods A gradient elution was performed on a mobile phase using a Thermo BDS Hypersil C8 column (2.1 mm × 100 mm, 2.4 μm) with 0.2% formic acid (A) and acetonitrile-methanol (6: 4, v / v) , And the flow rate was 0.3 mL · min-1. The results of multiple reaction monitoring (MRM) in the electrospray positive mode were as follows: m / z 129.9 → 70.9 (metformin), m / z 205.9 → 59.9 Biguanide), m / z 357.9 → 134.9 (rosiglitazone), m / z 494.0 → 169.0 (glibenclamide). Results Four hypoglycemic chemicals were detected at the same time. The detection limits were 0.06-0.5 ng · mL-1, and the limits of quantification were 0.21-1.62 ng · mL-1. The average recoveries of four chemicals were 66.3% -110.2% at the three different concentrations. The relative standard deviation (RSD) was 2.3% ~ 12.2%. Conclusion The method can detect four kinds of hypoglycemic agents illegally added to metformin, phenformin, rosiglitazone and glibenclamide in health food with high specificity and high sensitivity.