[1]王馨蔷,张文圣,陈兆杰,等.线硫醚在水、土壤及2种蔬菜中的残留检测方法[J].南京农业大学学报,2019,42(6):1067-1072.[doi:10.7685/jnau.201905019]
 WANG Xinqiang,ZHANG Wensheng,CHEN Zhaojie,et al.Determination method of exianliumi residues in water,soil and two kinds of vegetables[J].Journal of Nanjing Agricultural University,2019,42(6):1067-1072.[doi:10.7685/jnau.201905019]
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线硫醚在水、土壤及2种蔬菜中的残留检测方法()
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《南京农业大学学报》[ISSN:1000-2030/CN:32-1148/S]

卷:
42卷
期数:
2019年6期
页码:
1067-1072
栏目:
植物科学
出版日期:
2019-11-15

文章信息/Info

Title:
Determination method of exianliumi residues in water,soil and two kinds of vegetables
作者:
王馨蔷 张文圣 陈兆杰 朱椿元 熊伟宏 杨红
南京农业大学理学院/江苏省农药学重点实验室, 江苏 南京 210095
Author(s):
WANG Xinqiang ZHANG Wensheng CHEN Zhaojie ZHU Chunyuan XIONG Weihong YANG Hong
College of Sciences/Jiangsu Key Laboratory of Pesticide Science, Nanjing Agricultural University, Nanjing 210095, China
关键词:
线硫醚残留检测高效液相色谱样品净化
Keywords:
exianliumiresidue determinationHPLCsample purification
分类号:
O657.71;TQ450.263
DOI:
10.7685/jnau.201905019
摘要:
[目的] 本文旨在建立线硫醚在水、土壤、黄瓜和辣椒中的残留检测方法。[方法] 水样中线硫醚用LC-18固相萃取小柱提取、富集;土壤样品采用丙酮和水(体积比为3:1)超声提取,LC-18固相萃取小柱净化;辣椒样品匀浆后用丙酮超声提取,石油醚萃取净化;黄瓜样品匀浆后用丙酮超声提取时加微量甲酸,石油醚萃取,50 mg N-丙基乙二胺(primary secondary amine,PSA)净化。经前处理的所有样品均采用高效液相色谱-紫外检测器进行定量检测。[结果] 高效液相色谱法检测线硫醚,在0.01~10.00 mg·L-1内线性关系良好,相关系数(R2)为0.999 8,仪器最低检出限为0.01 mg·L-1。在试验添加浓度范围内,水中线硫醚的平均添加回收率为97.38%~100.25%,相对标准偏差(RSD)为1.22%~2.40%;土壤中线硫醚的加标平均回收率为92.73%~103.87%,RSD为2.21%~5.63%;黄瓜中线硫醚的加标平均回收率为91.83%~103.91%,RSD为1.11%~6.24%;辣椒中线硫醚的加标平均回收率为91.06%~106.29%,RSD为0.72%~6.76%。[结论] 建立的环境介质和2种蔬菜中线硫醚的残留检测方法,其准确度和精密度均能满足环境中农药残留分析的要求。
Abstract:
[Objectives] The purpose of this study was to report the analytical method of exianliumi residues in water,soil,cucumbers and hot peppers.[Methods] Exianliumi residue in water was extracted,preconcentrated and purified by LC-18 solid phase extraction(SPE). Soil was extracted by acetone-water(3:1,V/V),and purified by LC-18 SPE. Hot pepper samples were extracted with acetone and purified by petroleum ether. Cucumber samples were extracted with acetone added with a little of fomic acid,petroleum ether and then purified by adding 50 mg primary secondary amine(PSA). Exianliumi residues in four different kinds of samples were detected by high performance liquid chromatography with ultraviolet detector(HPLC-UVD).[Results] Exianliumi was determined by HPLC in the range of 0.01 to 10.00 mg·L-1,with the correlation coefficients(R2)being 0.999 8 respectively. The minimum detection limit of the instrument is 0.01 mg·L-1. The spiked recoveries of exianliumi in water ranged from 97.38% to 100.25% with the relative standard deviations(RSD)of 1.22%-2.40%,the soil sample from 92.73% to 103.87% with RSD of 2.21%-5.63%,the cucumber sample from 91.83% to 103.91% with RSD of 1.11%-6.24%,and the hot pepper sample from 91.06% to 106.29% with RSD of 0.72%-6.76%.[Conclusions] The analytical method of exianliumi residues in environmental media and two kinds of vegetables has the accuracy and precision to meet the requirements of pesticide residue analysis in the environment.

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备注/Memo

备注/Memo:
收稿日期:2019-05-13。
基金项目:国家重点研发计划项目(2018YFD0200100)
作者简介:王馨蔷,硕士研究生。
通信作者:杨红,教授,博导,研究方向为农药残留与环境毒理,E-mail:hongyang@njau.edu.cn。
更新日期/Last Update: 1900-01-01