分散固相萃取-UPLC-MS/MS法测定水蛭中10种磺胺类药物残留

Simultaneous Determination of Ten Kinds of Sulfonamide Residues in Leeches by DSPE-UPLC-MS/MS

目的建立分散固相萃取结合超高效液相色谱-串联质谱法测定中药材水蛭中10种磺胺类药物残留量的分析方法。方法比较不同提取溶剂与不同组合分散固相萃取填料的净化效果,以乙腈为提取溶剂,以100mg PSA、150mg C_(18)、900 mg MgSO4组合净化,采用电喷雾正离子MRM扫描模式检测,C_(18)色谱柱(1.7μm,2.1 mm×100 mm)分离,以含0.1%甲酸-2 mmol/l乙酸铵-水作为水相,含0.1%甲酸-乙腈作为有机相,梯度洗脱,外标法定量。结果10种磺胺类药物在各自线性范围内呈良好的线性关系,决定系数(R^(2))均大于0.99,检出限为0.19~1.16μg/kg,定量限为0.56~3.95μg/kg,3个加标水平的平均回收率为65.2%~98.0%,日内相对标准偏差为1.9%~8.3%,日间相对标准偏差为3.5%~9.2%。结论此法可用于快速、准确地筛查水蛭中10种磺胺类药物残留。

Objective To determine ten kinds of sulfonamides residues in leeches by dispersive solid-phase extraction(DSPE)combined with ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).Methods The purification effect of different extraction solvents and different combinations of DSPE were compared,and ultimately acetonitrile was chosen as extraction solvent and the combination 100 mg PSA,C_(18)150 mg and 900 mg MgSO4 were taken as cleaner.The electrospray positive ionization and of MRM scanning mode was used for detection.A C_(18) column(1.7μm,2.1 mm×100 mm)was used for the separation,and gradient elution was carried out with 0.1%formic acid-2 mmol/L ammonium acetate aqueous solution and acetonitrile solution containing 0.1%formic acid as mobile phases.The external standard method was used for quantification.Results Ten kinds of sulfonamides showed good linearities in their respective linear ranges.The determination coefficients(R^(2))were all greater than 0.99,the detection of limits were 0.19-1.16μg/kg,and the limits of quantitation were 0.56-3.95μg/kg.The recoveries of three spiked levels ranged from 65.2%to 98.0%,the relative standard deviations of intra-day precision ranged from 1.9%to 8.3%,and the relative standard deviations of inter-day precision ranged from 3.5%to 9.2%.Conclusion This method can be used for the rapid and accurate screening of ten kinds of sulfonamide residues in leeches.