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

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