Abstract: A high performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS) method was established for the simultaneous determination of six sulfonylurea drugs (gliquidone, glidenclamide, glimepiride, glipizide, glicianide and 1-butyl-3-(p-tolylsulfonyl)-urea) in milk powder claimed to have antidiabetic potency. After the sample was dissolved in warm water, the proteins were precipitated with zinc acetate and potassium ferrocyanide. The supernatant was separated on a Poroshell SB-C18 column, detected by HPLC-MS/MS under the multiple reaction monitoring (MRM) mode, and quantified by the external standard method. Under the optimized conditions, the six sulfonylurea drugs showed good linearity in the concentration range of 0.5–50.0 μg/L with correlation coefficients larger than 0.996. The detection limits of the method were 3.0 μg/kg for the six sulfonylurea drugs. The mean recoveries were in the range of 80.3%–95.5 % with relative standard deviations (RSDs, n = 6) ranging from 4.2% to 8.7%. The method had the advantages of high sensitivity, good purification effect and high quantitative accuracy, and was suitable for the detection of sulfonylurea drugs in antidiabetic milk powder.

Key words: high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS); sulfonylureas; milk powder; blood glucose

摘要： 建立一种同时测定血糖调节乳粉中6 种非法添加的磺酰脲类降血糖药物（甲苯磺丁脲、格列吡嗪、格列齐特、格列本脲、格列美脲和格列喹酮）的高效液相色谱-串联质谱分析方法。乳粉样品经温水溶解后，用亚铁氰化钾和乙酸锌沉淀蛋白质等物质，上清液过滤后采用Poroshell SB-C18色谱柱分离，多反应监测模式检测，外标法定量。结果表明：在最优实验条件下，6 种磺酰脲类化合物在0.5～50.0 μg/L范围内线性关系良好，R2均大于0.996，方法的检出限均为3.0 μg/kg；6 种化合物的回收率为80.3%～95.5

关键词: 高效液相色谱-串联质谱法；磺酰脲类化合物；乳粉；血糖