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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。
A liquid chromatography-mass spectrometry / mass spectrometry (LC-MS / MS) method was developed for the rapid determination of potent ether residues in six kinds of foods such as fruits, vegetables, grains, oilseeds, animal and plant fats and animal- The sample was salted-out and dehydrated, extracted with chloroform, cleaned up with Florisil silica solid phase extraction cartridge and eluted with acetone-chloroform mixed solvent. Acetonitrile-0.1% formic acid was used as the mobile phase, and Zobax SB C18 The liquid chromatographic column was separated and determined by mass spectrometry in electrospray positive ion multiple reaction monitoring mode. The effects of extraction solvent, purification method, column capacity, instrument conditions and matrix effect on the analytical results were investigated. The concentration of piperine in the range of 0.5 ~ 100μg / L, the linear correlation coefficient (r) was 0.9976, and the limit of quantification (LOQ) was 10μg / kg. The recoveries of four kinds of foodstuffs with LOQ, low MRL, 2 times MRL and high MRL were between 80.3% and 96.3% with relative standard deviations of 2.7% ~ 14%. The method could meet the needs of many kinds of food Qualitative and quantitative detection of potent ether residues in matrix.