| 超高效液相色谱-串联质谱法测定莲藕、莲叶、莲子、田泥与田水中12种农药残留 |
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| 基金项目:农业部标准制定和农药残留登记试验项目（2015H012）；国家自然科学基金资助项目（31772077） |
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| 中文摘要:建立了莲藕、莲叶、莲子肉、莲子壳、田泥和田水中12种农药残留的分析方法。固体样品采用乙腈-水混合提取，氯化钠盐析后离心，分取乙腈提取液过PestiCarb固相萃取柱净化洗脱，水样采用C18固相萃取柱直接富集净化洗脱，洗脱液浓缩定容后经超高效液相色谱-串联质谱（UPLC-MS/MS）基质外标法定量，并对12种农药的质谱裂解、基质效应进行了探讨。12种农药在0005（0010）~2500 mg/L范围内均呈线性关系，相关系数（r2）大于097；在低、中、高加标浓度下，莲叶、莲藕、莲子肉和莲子壳中12种化合物的平均加标回收率（AR）为756%~116%，相对标准偏差（RSD）为13%~251%;田泥中除咪鲜胺之外，其余化合物的AR为646%~104%，RSD为09%~95%;田水中除噻虫胺在低浓度、咪鲜胺和茚虫威在中、高加标浓度下的AR＜70%外，其余化合物的AR为712%~101%，RSD为09%~169%。除田水中噻虫胺外，其余方法定量下限均不大于001 mg/kg和01 μg/L。采用该法进行了莲藕田撒施10%异草松·异丙甲草胺·扑草净颗粒剂后的最终残留试验，结果表明：以有效成分剂量630 g ai/ha和945 g ai/ha施用1次后，异草松和异丙甲草胺在莲藕、莲子和莲叶中均无残留，扑草净在莲藕、莲子壳、莲子肉和莲叶样品中的残留量分别不超过0022、0166、0012、0181 mg/kg。 |
| 中文关键词:农药多残留分析 超高效液相色-串联质谱法（UPLC-MS/MS） 莲藕 莲子 |
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| Simultaneous Determination of 12 Pesticides in Root,Leaf and Seed of Lotus,Mud and Field Water by Ultrahigh Performance Liquid Chromatography-Tandem Mass Spectrometry |
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| Abstract:A sensitive and convenient method was established for the analysis of twelve kinds of pesticide in root,leaf,seed meat and seed shell of lotus,mud and field water by ultrahigh performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS）.The solid samples were extracted with acetonitrile/water,then salted out with sodium chloride and following by a centrifugal separation,finally purified and eluted with a PestiCarb-SPE column.The water samples were simply enriched,cleaned up and eluted with a BondElut C18-SPE column.The eluted fractions were analyzed by UPLC-MS/MS,and quantified by the matrix external standard method.The mass fragmentation pathway and matrix effect of twelve pesticides were also investigated.The calibration curves for the target compounds were linear in the concentration range of 0005（0010）-2500 mg/L,with their correlation coefficients（r2） more than 097.The average recoveries（AR） for twelve pesticides at high,middle and low spiked levels in lotus leaf,root,seed and seed shell were between 756% and 116%,with relative standard deviations（RSDs） of 13%-251%,while the AR.for other eleven pesticides except prochloraz in mud were 646%-104% with RSDs of 09%-95%;Besides,the AR.for the analytes in field water ranged from 712% to 101% with RSDs of 09%-169%,except that the AR.for clothianidin at low level,prochloraz and indoxacarb at middle and low levels were less than 70%.The limits of quantitation（LOQs） of this method were not more than 001 mg/kg and 01 μg/L,except clothianidin.After 10% clomazone-metolachlor-prometryne granules were spread into the lotus root fields by dosages of 630 g ai/ha and 945 g ai/ha in one time,final residue test was investigated by this method.Results showed that there were no clomazone and metolachlor residues in lotus root,lotus seed and lotus leaf samples,and the residual amounts of prometryne were not more than 0022,0166,0012 and 0181 mg/kg in the lotus root,lotus seed shell,lotus seed meat and lotus leaf samples,respectively. |
| Key Words:multi pesticide residue analysis ultrahigh performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS） lotus root lotus seed |
| 引用本文：张新忠,陈宗懋,赵梅勤,姚月凤,绳慧珊,王新茹,周利,罗逢健.超高效液相色谱-串联质谱法测定莲藕、莲叶、莲子、田泥与田水中12种农药残留[J].分析测试学报,2018,37(10):1221-1229. |
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