色谱2012，Vol.30Issue(9)：962-965,4.DOI:10.3724/SP.J.1123.2012.06008
液相色谱-串联质谱法测定蔬菜和水果中硝苯菌酯的残留量
Determination of meptyldinocap residues in vegetable and fruit by liquid chromatography-tandem mass spectrometry
摘要
Abstract
A method was developed for the determination of the residues of meptyldinocap (2,4-dinitro-6-( 1-methylheptyl) phenyl crotonate, 2,4-DNOPC) as 2, 4-dinitrooctylphenol (2,4-dinitro-6-( 1-methylheptyl) phenol, 2,4-DNOP), which is a hydrolysate of 2,4-DNOPC, in six vegetable and fruit by using liquid chromatography coupled with electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS). The residues of 2,4-DNOPC in vegetable and fruit samples were extracted by the mixture of acetone, methanol and hydrochloric acid, then extracted by liquid-liquid partitioning, hydrolyzed under alkaline condition with ultrasonication, and extracted again by liquid-liquid partitioning, then analyzed by using LC-MS/MS in multiple reaction monitoring (MRM) mode via negative electrospray ionization with an Agilent ZORBAX SB-C18 column. The method was validated at four fortification levels in vegetable and fruit. The validation results were as follows: the recoveries of 2,4-DNOPC in cabbages were from 89.7% to 93. 3% (the relative standard deviations (RSD) of 6. 3% - 8. 5%), in cucumbers from 87. 7% to 95.1% (RSD of 5. 8% - 10.4%), in tomatoes from 89. 3% to 96. 0% (RSD of 6. 8% - 9. 2%), in apples from 92.0% to 98. 3% (RSD of 5. 1 % - 10. 3%), in pears from 89. 0% to 95. 0% (RSD of 5. 3% - 10. 2%), in grapes from 81.2% to 95. 8% ( RSD of 5. 8% - 10.4%). The limits ofquantification of 2,4-DNOPC in all the test samples were 0. 01 mg/kg. The results showed that the method is simple, rapid, and is characterized with acceptable sensitivity and accuracy to meet the requirements of the pesticide residue analysis. This method is applicable to confirm the residues of meptyldinocap in vegetable and fruit samples.关键词
液相色谱-串联质谱/硝苯菌酯/蔬菜/水果Key words
liquid chromatography-tandem mass spectrometry (LC-MS/MS)/ meptyldinocap/vegetable/ fruit分类
化学化工引用本文复制引用
张志勇,单炜力,简秋,段丽芳,沈燕,刘贤金..液相色谱-串联质谱法测定蔬菜和水果中硝苯菌酯的残留量[J].色谱,2012,30(9):962-965,4.基金项目
江苏省农业科技自主创新资金项目(CX(11)4069) （CX(11）
