超高效液相色谱-串联质谱法测定环境样品中溴嘧氯草醚残留及其在土壤中降解特性的研究

建立了超高效液相色谱-串联质谱法（UPLC-MS/MS）测定土壤、沉积物和水中溴嘧氯草醚残留量的方法,研究了溴嘧氯草醚在3种不同类型土壤中的降解特性。样品经乙腈提取后,以C_（18）固相萃取柱净化,采用梯度洗脱程序、BEH C_（18）色谱分离柱、应用UPLC-MS/MS多反应监测模式测定溴嘧氯草醚。对0.005、0.05和2.0 mg/kg添加浓度样品进行回收实验,溴嘧氯草醚在土壤、沉积物和水中的平均回收率为87%~106%,变异系数为2.8%~8.0%。溴嘧氯草醚在0.5~20μg/L浓度范围内相关系数R~2〉0.9999,溴嘧氯草醚在土壤（沉积物）和水中的定量限分别为0.2μg/kg和0...

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Bibliographic Details
Published in分析化学 Vol. 45; no. 10; pp. 1564 - 1570
Main Author 何红梅 吴珉 张春荣 俞建忠 赵华 朱亚红 何开雨 张昌朋 蔡磊明 徐玲英 唐庆红
Format Journal Article
LanguageChinese
Published 省部共建国家重点实验室培育基地"浙江省植物有害生物防控重点实验室",农业部农药残留检测重点实验室,浙江省农业科学院农产品质量标准研究所,杭州310021%中国科学院上海有机化学研究所,上海,200032 2017
Subjects
土壤降解
残留
液相色谱-串联质谱
溴嘧氯草醚
土壤降解
残留
4-Bromo-N-( 2-chloro-6-
Residue
液相色谱-串联质谱
6-dimethoxypyrimidin-2-yloxy ) benzyl ) aniline
Soil degradation
Ultra performance liquid chromatography-tandem mass spectrometry
溴嘧氯草醚
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ISSN0253-3820
DOI10.11895/j.issn.0253-3820.170338

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Summary:建立了超高效液相色谱-串联质谱法（UPLC-MS/MS）测定土壤、沉积物和水中溴嘧氯草醚残留量的方法,研究了溴嘧氯草醚在3种不同类型土壤中的降解特性。样品经乙腈提取后,以C_（18）固相萃取柱净化,采用梯度洗脱程序、BEH C_（18）色谱分离柱、应用UPLC-MS/MS多反应监测模式测定溴嘧氯草醚。对0.005、0.05和2.0 mg/kg添加浓度样品进行回收实验,溴嘧氯草醚在土壤、沉积物和水中的平均回收率为87%~106%,变异系数为2.8%~8.0%。溴嘧氯草醚在0.5~20μg/L浓度范围内相关系数R~2〉0.9999,溴嘧氯草醚在土壤（沉积物）和水中的定量限分别为0.2μg/kg和0.2μg/L。应用建立的溴嘧氯草醚残留分析方法检测了土壤降解样品,结果表明,溴嘧氯草醚在3种不同土壤中好氧降解的半衰期为1.72~28.2 d,厌氧降解的半衰期为2.93~31.4 d;在同一种土壤样品中,好氧条件下溴嘧氯草醚降解快于厌氧条件;土壤中溴嘧氯草醚降解的快慢与土壤的pH值、阳离子交换量和土壤质地有关。
Bibliography:HE Hong-Mei1 , WU Min1 , ZHANG Chun-Rong1 , YU Jian-Zhong1 , ZHAO Hua1 , ZHU Ya-Hong1 , HE Kai-Yu1 , ZHANG Chang-Peng1, CAI Lei-Ming1, XU Ling-Ying1, TANG Qing-Hong2 （ 1State Key Lab Breeding Base for Zhejiang Sustainable Plant Pest Control, MOA Key Lab for Pesticide Residue Detection ; Institute f Quality and Standard for Agro-products, Zhejiang Academy f Agricultural Sciences, Hangzhou 310021, China ;2 Shanghai Institute of Organic Chemistry, Chinese Academy of Sciences, Shanghai 200032, China）
An analytical method based on ultra performance liquid chromatography-tandem mass spectrometry was developed for the determination of SIOC0426 residues in environment samples（soil,sediment and water）.The fate of SIOC0426 in three kinds of soils was also evaluated.The target compound was extracted with acetonitrile,cleaned up by C_（18） cartridge,and analyzed by gradient ultra performance liquid chromatographytandem mass spectrometry with electrospray ionization under positive mode（ESI ＋） using a UPLC BEH C_（18） column.
ISSN:0253-3820
DOI:10.11895/j.issn.0253-3820.170338