液相色谱-质谱联用法测定猪肉中16种磺胺类药物的残留

Determination of 16 kinds of sulfonamides residues in pork by liquid chromatogram-mass spectrometry

采用液相色谱-质谱联用仪建立了同时测定16种磺胺类药物残留的分析方法。样品中的残留经乙腈提取,离心提取,上清液用旋转蒸发仪蒸发浓缩至近干,残渣用流动相溶解,并用正己烷脱脂净化后,采用色谱柱分离,以0.1%甲酸-水溶液作为流动相,进行梯度洗脱,目标分析物在多反应监测模式下包留时间和离子对进行定向分析,外标法测定。12min完成分析。16种化合物在测定范围内线性关系良好(R>0.99),在两个加标水平下,回收率为80.8%~98.7%,相对标准差(RSD<10%),该分析方法时间短、选择性好、灵敏度高,可以满足猪肉中16种磺胺的测定。

The liquid chromatogram - mass spectrometry was adopted, and the analytical method of determining 16 kinds of sulfonamides residues simultaneously was established. The residues of samples were extracted by acetonitrile and centrifugation, supernatant was evaporated and concentrated to near dry by rotary evaporator, residues were dissolved by mobile phase, and it was defatted and purified by n - hexane. It was separated by column, 0.1% formic acid - water was taken as mobile phase, gradient elution was conducted, orientation analysis of retention time and ion pair of target analyte was conducted in multiple reaction monitoring mode, and it was determined by external standard method. The analysis could be completed in 12 min. The linear relationship of 16 kinds of compounds in the determination range was good （R 〉 0.99）, and the recovery rate was 80.8% - 98.7%, and the relative standard deviations （ RSD 〈 10% ） were obtained at the two spiked levels. The time was short, the selectivity was good and the sensitivity was high of this analysis method and it could meet the determination of 16 kinds of sulfonamides in pork.