食品科学2018，Vol.39Issue(8)：302-308,7.DOI:10.7506/spkx1002-6630-201808047
超高效液相色谱-串联质谱法测定果蔬中氟啶虫胺腈、Pyrifluquinazon和螺虫乙酯残留量
Determination of Sulfoxaflor, Pyrifluquinazon and Spirotetramat Residues in Fruits and Vegetables by UPLC-MS/MS
摘要
Abstract
In this study, a rapid, highly sensitive and selective method was developed for the simultaneous determination of residues of sulfoxaflor, pyrifluquinazon and spirotetramat in fruits (apple, grape, and strawberry) and vegetables (cucumber, onion, Chinese cabbage, spinach, and welsh onion) by ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The target compounds were extracted from the samples with acetonitrile and cleaned up with dispersive solid phase extraction using primary secondary amine (PSA) and C18as solid phase before being separated on a C18 column. Two pairs of precursor product ion transitions for sulfoxaflor, pyrifluquinazon and spirotetramat were measured and evaluated under the positive multiple reaction monitoring (MRM) mode. Matrix effects were tested by comparison of reference standards in pure solvent with matrix-matched standards of each matrix. In order to reduce the systematic error, quantification was performed using matrix-matched standard calibration curves. Satisfactory linearity in the concentration range of 0.2-100, 0.02-10 and 0.1-10 μg/L for sulfoxaflor, pyrifluquinazon and spirotetramat, respectively were obtained with correlation coefficients (r) of higher than 0.999 0. Average recoveries of sulfoxaflor, pyrifluquinazon and spirotetramat added to cucumber, grape, apple and scallion ranged from 79.9% to 103.9%, with relative standard deviations (RSD) from 3.3% to 8.8%. The limits of quantification (LOQs) were 0.334, 0.040 5 and 0.378 μg/kg, and the limits of detection (LODs) were 0.100, 0.012 2 and 0.133 μg/kg for sulfoxaflor, pyrifluquinazon and spirotetramat respectively. The method is quick, easy, effective, sensitive and accurate, and can meet the requirements for the determination of residues of sulfoxaflor, pyrifluquinazon and spirotetramat in fruits and vegetables.关键词
超高效液相色谱-串联质谱/果蔬/Pyrifluquinazon/氟啶虫胺腈/螺虫乙酯/残留Key words
ultra performance liquid chromatography-tandam mass spectrometry (UPLC-MS/MS)/fruits and vegetables/pyrifluquinazon/sulfoxaflor/spirotetramat/residues分类
化学化工引用本文复制引用
崔淑华,李正义,程刚,李瑞娟,王宇,张雪琰,赵峰..超高效液相色谱-串联质谱法测定果蔬中氟啶虫胺腈、Pyrifluquinazon和螺虫乙酯残留量[J].食品科学,2018,39(8):302-308,7.基金项目
山东出入境检验检疫局科研项目(SK201425) （SK201425）
