高效液相色谱-串联质谱法快速测定6类食品中增效醚的残留

建立了水果、蔬菜、粮谷、油料、动植物脂类、动物源性食品等6类食品中增效醚残留量快速测定的液相色谱-质谱/质谱(LC-MS/MS)方法。样品盐析并除水后,用三氯甲烷提取,氟罗里硅土填料固相萃取柱净化,丙酮-三氯甲烷混合溶剂洗脱,以乙腈-0.1%甲酸为流动相,在Zobax SB C18液相色谱柱完成分离,并于电喷雾正离子多反应监测模式下质谱测定。考察了提取溶剂、净化方法、柱容量、仪器条件、基质效应对分析结果的影响。增效醚质量浓度在0.5～100μg/L范围内,线性相关系数(r)为0.9976,方法定量限(LOQ)为10μg/kg。17种食品基质添加LOQ、低MRL、2倍MRL、高MRL 4个不同浓度水平时,回收率在80.3%～96.3%之间,相对标准偏差为2.7%～14%,方法可以满足多种食品基质中增效醚残留量的定性和定量检测要求。

Rapid determination of piperonyl butoxide residues in 6 kinds foodstuffs with high performance liquid chromatography tandem mass spectrometry

A rapid confirmative method was developed for the determination of piperonyl butoxide residues in 6 kinds of foodstuffs,such as fruits,vegetables,cereals,oilseeds,animal and vegetable oils,animal-origin foods by liquid chromatography tandem mass spectrometry(LC-MS/MS).After salted-out and removed-water,the sample was extracted with chloroform,then clean-up procedure was selected with florisil solid-phase extraction (SPE) and the analyte were eluted with acetone-chloroform solvent.The separation was performed on a Zobax SB C18 column with the mobile phase of acetonitrile-0.1% formic acid.The piperonyl butoxide was analyzed quantitatively by mass spectrometry with positive electrospray ionization(ESI +) multiple reaction monitoring (MRM) mode.The influence factors including extraction,purification,column capacity,chromatographic or mass spectrometric conditions,and matrix effects were optimized.With the linearity in the range of 0.5-100 μg/L,the obtained r value was 0.9976.The limit of quantification was 10 μg/kg.The method recoveries varied from 80.3% to 96.3% and the relative standard deviations(RSD) were between 2.7% and 14%.The validated method was simple,fast,sensitive,and was satisfactory with requirements of detection of piperonyl butoxide residues in various food matrices.