| 路彩红1, 杨林1, 申流柱1, 刘路1, 姚赛1, 吴希1, 张盈2, 段婷婷2*.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[J].植物保护,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 |
| Residues and degradation determination of fluxapyroxad inrice and soil by UPLC-MS/MS |
| 投稿时间：2015-07-12 修订日期：2015-09-06 |
| DOI： |
| 中文关键词: 氟唑菌酰胺 水稻 土壤；UPLC-MS/MS 残留 |
| 英文关键词:fluxapyroxad rice soil UPLC-MS/MS residue |
| 基金项目:贵州省自然科学基金（［2015］2101号） |
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| 全文下载次数: 1986 |
| 中文摘要: |
| 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1 mg/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3.21 μg/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9.9 d, 表明氟唑菌酰胺属于易降解农药。 |
| 英文摘要: |
| 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 and 1.0 mg/kg) ranged from 82.7% to 111.7% 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 3.21 μg/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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