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当前位置: 首页 > 文章 > 超高效液相色谱-串联质谱法检测水稻和土壤中氟唑菌酰胺的残留及消解动态 植物保护 2016,42 (4) 132-136
Position: Home > Articles > Residues and degradation determination of fluxapyroxad in rice and soil by UPLC-MS/MS Plant Protection 2016,42 (4) 132-136

超高效液相色谱-串联质谱法检测水稻和土壤中氟唑菌酰胺的残留及消解动态

作  者：
路彩红;杨林;申流柱;刘路;姚赛;吴希;张盈;段婷婷
单  位：
贵州省毕节市农产品质量安全监督检验测试中心;贵州省农业科学院植物保护研究所
关键词：
氟唑菌酰胺;水稻;土壤;UPLC-MS/MS;残留
摘  要：
本文采用QuEChERS方法,建立了超高效液相色谱-串联质谱(UPLC-MS/MS)快速测定氟唑菌酰胺在水稻糙米、水稻壳、水稻植株、稻田水和土壤样品中的残留分析方法。样品经乙腈提取,十八烷基硅烷键合硅胶(C18)、石墨化炭黑(GCB)和N-丙基乙二胺(PSA)净化后采用外标法进行定量分析。添加浓度为0.1、0.5和1mg/kg时,氟唑菌酰胺在水稻植株、土壤、糙米、稻壳和稻田水中的平均回收率为82.7%~111.7%,变异系数为1.6%~13.0%,氟唑菌酰胺在水稻植株、土壤、糙米、稻壳和稻田水中的最低检出浓度LOQs分别是18.89、2.85、10.27、30.21和3.21μg/kg。该方法的准确度和精密度等均符合农药残留分析的要求。田间试验结果表明,氟唑菌酰胺在水稻植株中的消解动态符合一级动力学方程,安徽、广西和北京三地的水稻植株上的消解半衰期分别为2.5、3.8和9.9d,表明氟唑菌酰胺属于易降解农药。
译  名：
Residues and degradation determination of fluxapyroxad in rice and soil by UPLC-MS/MS
作  者：
Lu Caihong;Yang Lin;Shen Liuzhu;Liu Lu;Yao Sai;Wu Xi;Zhang Ying;Duan Tingting;Bijie Supervision and Testing Center of Agricultural Products Quality &Safety;Institute of Plant Protection,Guizhou Academy of Agricultural Sciences;
关键词：
fluxapyroxad;;rice;;soil;;UPLC-MS/MS;;residue
摘  要：
A rapid,highly sensitive and selective method was developed for determination of fluxapyroxad by QuEChERS coupled with ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The target compound was extracted with acetonitrile,and cleaned up with primary secondary amine(PSA),graphitized carbon black(GCB)or octadecylsilane(C18).Average recoveries for rice plant,paddy soil,brown rice,rice hull and water at three spike levels(0.1,0.5 and1.0mg/kg)ranged from82.7%to111.7% with coefficients of variation of 1.6%to 13.0%,and the limit of quantifications(LOQs)were 18.89,2.85,10.27,30.21 and 3.21μg/kg,respectively.Therefore,the established method was suitable for the determination of fluxapyroxad residues in rice.The field experiments demonstrated that the degradation of fluxapyroxad in rice plant was conformed to the first-order dynamic equation.The results showed that the half-lives of fluxapyroxad were 2.5,3.8 and 9.9 days in rice plants from Anhui,Guangxi and Beijing,indicating that fluxapyroxad was easily degradable in the rice eco-system.

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