超高效液相色谱-串联质谱法同时测定水果中9种杀菌剂的残留量

Simultaneous determination of 9 fungicide residues in fruits by UPLC-MS / MS

目的建立一种同时测定水果中9种杀菌剂残留的超高效液相色谱-串联质谱分析方法。方法样品经乙腈超声提取,离心后取上清液过固相萃取柱净化,通过ACQUITY UPLC HSS T3色谱柱分离,以乙腈-0.05%甲酸水作为流动相进行梯度洗脱,采用多反应监测(MRM)模式,以外标法定量。结果 9种杀菌剂的质量浓度为20 ng/ml^1 000 ng/ml时,线性关系良好,相关系数(r)≥0.995 0,检出限为0.4μg/kg^2.0μg/kg。方法的平均回收率为83.2%~101.0%,相对标准偏差(RSD)为2.3%~6.6%。结论该方法具有灵敏度高、样品前处理简单、分析时间短等优点,可满足水果中9种常见杀菌剂的检测要求。

Objective An ultra - performance liquid chromatography - tandem mass spectrometric method （ UPLC - MS/MS） was established for the simultaneous determination of 9 fungicide residues in fruits. Methods The fungicide residues in sam- ples were extracted by acetonitrile. After centrifugation, the supernatant was cleaned up by solid phase extraction column. Tar- get compounds, which were separated on a HSS T3 column using acetonitrile -0.05% formic acid as mobile phase, were identi- fied in multiple reaction monitoring mode（MRM） and quantified by external standard method. Results The calibration curves for the nine fungicides were linear in the range of 20 ng/ml - 1 000 ng/ml with the correlation coefficient （r） 90.995 0, and the detection limit of 0.4 ～g/kg- 2.0 p.g/kg, the spike recoveries were in the range of 83.2% -101.0% and the average re- covery rate of 2.3 % -6.6%. Conclusion The method has the advantages of high sensitivity, simple operation, rapid deter- mination, and can be suitable for the detection of nine common fungicides in fruits.