摘要
建立了QuEChERS-超高效液相色谱-串联质谱技术同时测定茶叶中氟唑磺隆和氟吡磺隆含量的快速检测方法。茶叶样品中的氟唑磺隆和氟吡磺隆残留经乙腈提取,以石墨化碳黑粉末吸附提取液中的杂质,提取液离心、过滤后经超高效液相色谱-串联质谱法测定,外标法定量。研究提取溶剂、吸附剂种类及用量对提取净化效率的影响。结果表明:在优化试验条件下,氟唑磺隆和氟吡磺隆在0.000 5 mg/L～0.05 mg/L范围内线性关系良好,相关系数(r)均大于0.998,氟唑磺隆和氟吡磺隆的方法定量限均为0.005 mg/kg。氟唑磺隆和氟吡磺隆在0.005、0.02、0.1 mg/kg加标水平下的平均回收率分别为92.8%～110.3%和85.2%～97.6%,相对标准偏差(n=6)分别为3.42%～9.27%和3.65%～10.35%;该方法操作简单、快速、灵敏、成本低,能满足茶叶中氟唑磺隆和氟吡磺隆的检测需求。
A rapid method for the simultaneous determination of flucarbazone-sodium and flucetosulfuron in tea was developed by ultra performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS)coupled with QuEChERS. Flucarbazone-sodium and flucetosulfuron residues in tea were extracted with acetonitrile,and cleaned up by graphitized carbon black powder as dispersive solid-phase extraction sorbent. After centrifugation and filtration,the target compounds were analyzed by ultra performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS)and quantified by the external standard method. Effects of different extraction solvents and sorbents,amount of graphitized carbon black powder on the determination of flucarbazone-sodium and flucetosulfuron were investigated. The results showed good linearities for flucarbazone-sodium and flucetosulfuron in the range of 0.000 5 mg/L-0.05 mg/L under the optimal conditions,the correlation coefficients(r)were greater than 0.998,and the quantitation limits of the method were 0.005 mg/kg both for flucarbazonesodium and flucetosulfuron. The mean spiked recoveries of flucarbazone-sodium and flucetosulfuron at three concentration levels of 0.005,0.02,0.1 mg/kg were in the range of 92.8 %-110.3 % and 85.2 %-97.6 %,with relative standard deviations(RSDs,n =6)of 3.42 %-9.27 % and 3.65 %-10.35 %. The method is simple,rapid,sensitive,and cheap,it could meet the requirements for the detection of flucarbazone-sodium and flucetosulfuron in tea.
引文
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