摘要
建立了一种通过检测硝苯菌酯(2,4-dinitro-6-(1-methylheptyl)phenyl crotonate,2,4-DNOPC)相应的水解产物2,4-二硝基-6-(1-甲基庚基)苯酚(2,4-dinitro-6-(1-methylheptyl)phenol,2,4-DNOP)来测定蔬菜和水果中2,4-DNOPC残留量的液相色谱-电喷雾串联质谱(LC-ESI-MS/MS)检测方法。蔬菜和水果样品用丙酮-甲醇-盐酸的混合液进行液-液分配提取,在碱性条件下超声水解后再进行液-液分配提取,然后进行LC-MS/MS测定。2,4-DNOPC在6种蔬菜和水果中的回收率试验结果表明,2,4-DNOPC在甘蓝中的添加回收率为89.7%~93.3%,相对标准偏差(RSD)为6.3%~8.5%;在黄瓜中的添加回收率为87.7%~95.1%,RSD为5.8%~10.4%;在番茄中的添加回收率为89.3%~96.0%,RSD为6.8%~9.2%;在苹果中的添加回收率为92.0%~98.3%,RSD为5.1%~10.3%;在梨中的添加回收率为89.0%~95.0%,RSD为5.3%~10.2%;在葡萄中的添加回收率为81.2%~95.8%,RSD为5.8%~10.4%。2,4-DNOPC在6种蔬菜和水果的最低检测浓度均为0.01 mg/kg。该检测方法样品前处理简单、快速,分析时间短,灵敏度、准确度和精密度均符合农药残留检测要求,适用于蔬菜和水果中硝苯菌酯残留量的检测。
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 of quantification 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.
出处
《色谱》
CAS
CSCD
北大核心
2012年第9期962-965,共4页
Chinese Journal of Chromatography
基金
江苏省农业科技自主创新资金项目(CX(11)4069)
关键词
液相色谱-串联质谱
硝苯菌酯
蔬菜
水果
liquid chromatography-tandem mass spectrometry(LC-MS/MS); meptyldinocap; vegetable; fruit