SPE净化-超高效液相色谱-串联质谱法测定水果中的多果定残留量

Determination of Dodine Residues in Fruits by SPE Purification Combined with Ultra Performance Liquid Chromatography Tandem Mass Spectrometry

建立了快速测定水果中超高效液相色谱-串联质谱法(Ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)测定水果中的多果定残留量。样品使用甲醇提取后,WCX固相萃取柱净化,经Xbridge BEH C18色谱柱(100 mm×4.6 mm,2.5μm)分离,最后经UPLC-MS/MS测定。多果定母离子及子离子碎片通过多反应监测模式(Multiple reaction monitoring,MRM)进行采集。多果定在1.0~100μg/L线性范围内,线性关系良好,相关系数R2为0.9994。在质量浓度为1.0、2.0、10.0μg/kg的添加水平下,加标回收率在89.1%~99.5%之间,相对标准偏差为2.98%~6.69%。以信噪比3倍和10倍确定的方法检出限为0.3μg/kg,方法定量限为1.0μg/kg。该方法回收率高,重现性好,灵敏度高,适用于水果中多果定的分析测定。

A rapid method was established for the determination of dodine residues in fruits by ultra performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS).After the sample was extracted with methanol and then purified by WCX solid phase extraction column and separated by Xbridge BEH C18 chromatographic column(100 mm×4.6 mm,2.5μm),finally determined by UPLC-MS/MS.The parent ion and daughter ion fragments of dodine were collected by multiple reaction monitoring(MRM).The linear relationship of dodine was good in the concentration range of 1.0~100μg/L with the correlation coefficient R2 was 0.9994.At the addition level of 1.0,2.0,10.0μg/kg,the recoveries were 89.1%~99.5%,while the relative standard deviations(RSDs)were in the range of 2.98%~6.69%.The detection limit and quantitation limit of the method determined by 3 times and 10 times of the signal-to-noise ratio was 0.3μg/kg and 1.0μg/kg respectively.The method has high recovery,good reproducibility and high sensitivity that indicated it was suitable for the analysis and determination of dodine in fruits.