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水稻和土壤中呋虫胺残留的固相萃取/液相色谱-串联质谱分析方法

Analytical Method for Determination of Dinotefuran Residues in Rice and Soil by SPE/HPLC- MS/MS

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【作者】 王冬兰简秋郑尊涛宋稳成孙星朱宏杨邦保

【Author】 WANG Dong-lan;JIAN Qiu;ZHENG Zun-tao;SONG Wen-cheng;SUN Xing;ZHU Hong;YANG Bang-bao;Key Laboratory of Control Technology and Standard for Agro-product Safety and Quality,Ministry of Agriculture,P.R.China , Key Lab of Agro-product Safety Risk Evaluation(Nanjing) ,Ministry of Agriculture;Institute for the Control of Agrochemicals,Ministry of Agriculture;

【机构】 农业部农产品质量安全控制技术与标准重点实验室/农业部农产品质量安全风险评估实验室(南京)农业部农药检定所

【摘要】 建立了呋虫胺在水稻(糙米、稻壳和稻草3种基质)和土壤中残留的液相色谱-电喷雾串联质谱(LC-ESI MS/MS)检测方法。各基质经乙腈提取,PSA柱净化后,以Agilent ZORBAX SB-C18色谱柱分离,电喷雾电离串联质谱正离子多重反应监测(MRM)模式进行测定。在不同加标水平下,对呋虫胺在4种不同基质中的回收率和相对标准偏差(RSD)进行测定。结果表明,呋虫胺在糙米中的回收率为73.8%~97.2%,RSD为3.1%~9.9%;在稻壳中的回收率为77.6%~80.3%,RSD为2.5%~5.8%;在稻草中的回收率为76.0%~94.0%,RSD为4.8%~8.8%;在土壤中的回收率为83.6%~93.3%,RSD为4.6%~6.4%。该方法具有样品前处理简单、快速、分析时间短的特点,灵敏度、准确度和精密度均符合农药残留检测要求。

【Abstract】 A simple and sensitive method was developed for the determination of dinotefuran residues in brown rice,hull,straw and soil. The residues of dinotefuran in different matrix were extracted with acetonitrile. After cleaned with PSA column,the extract was separated on an Agilent ZORBAX SB- C18 analytical column,and determined by liquid chromatography- tandem mass spectrometry( LC- MS /MS) under multiple reaction monitoring( MRM) mode. The method was validated at different fortification levels in brown rice,hull,straw and soils. The recoveries for brown rice at three fortification levels ranged from 73. 8% to 97. 2% with relative standard deviations( RSDs) not more than 9. 9%. The recoveries for hull were between 77. 6% and 80. 3% with RSDs not more than5. 8%. The recoveries for straw were between 76. 0% and 94. 0% with RSDs not more than 8. 8%.The recoveries for soil were between 83. 6% and 93. 3% with RSDs not more than 6. 4%. The results showed that the method is simple and rapid,and its sensitivity and accuracy could meet the requirements for pesticide residue analysis.

【基金】 江苏省农业自主创新资金项目(CX(14)2060)
  • 【文献出处】 分析测试学报 ,Journal of Instrumental Analysis , 编辑部邮箱 ,2016年03期
  • 【分类号】X839.2;O657.63
  • 【被引频次】12
  • 【下载频次】299
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