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Supercritical fluid chromatographic-tandem mass spectrometry method for monitoring dissipation of thiacloprid in greenhouse vegetables and soil under different application modes
Journal of Chromatography B ( IF 3 ) Pub Date : 2018-02-16 , DOI: 10.1016/j.jchromb.2018.02.021
Runan Li , Zenglong Chen , Fengshou Dong , Jun Xu , Xingang Liu , Xiaohu Wu , Xinglu Pan , Yan Tao , Yongquan Zheng

A rapid, sensitive and effective supercritical fluid chromatographic-tandem mass spectrometry (SFC-MS/MS) method was developed to analyze thiacloprid for the first time. The SFC-MS/MS conditions were optimized with the ultra-performance convergence chromatography (UPC2) BEH column (100 mm × 3.0 mm, 1.7 μm particle size) and thiacloprid was eluted at 1.22 min in gradient mode with CO2/methanol as mobile phase. The 0.1% formic acid in methanol (v/v) was used as postcolumn compensation solution to improve sensitivity. The ABPR pressure, flow rate of mobile phase and flow rate of compensation pump were set at 1800 psi, 1.8 mL/min, and 0.1 mL/min, respectively. The average recoveries of thiacloprid in soil at four spiking levels (5, 10, 100, 1000 μg/kg) ranged between 78.8% and 107.1% with relative standard deviations (RSDs) lower than 12.2% and the limit of quantitation (LOQ) was 5 μg/kg. The proposed method can distinctly improve the analysis efficiency by 2–12 times and reduce the solvent consumption by 5%–95% compared with reported methods. It was applied to investigate the dissipation rates of thiacloprid in greenhouse vegetables and soil under different application modes. The half-lives of thiacloprid in cucumber and soil were 9.55–20.44 days and 3.74–9.14 days separately under different application modes, 10.60 days in tomato under foliar spraying. The residues in vegetables under root irrigation were all less than that under foliar spraying. The results could offer useful data for risk assessment of thiacloprid in agricultural production.



中文翻译:

超临界流体色谱-串联质谱法监测不同应用模式下温室蔬菜和土壤中噻虫啉的消散

建立了快速,灵敏,有效的超临界液相色谱-串联质谱(SFC-MS / MS)方法来首次分析噻虫啉。SFC-MS / MS条件通过超高效收敛色谱(UPC 2)BEH柱(100 mm×3.0 mm,粒径1.7μm)进行了优化,噻虫啉在1.22 min时以CO 2 /甲醇作为洗脱液洗脱。流动相。甲醇中的0.1%甲酸(v / v)用作柱后补偿溶液以提高灵敏度。ABPR压力,流动相流速和补偿泵流速分别设置为1800 psi,1.8 mL / min和0.1 mL / min。四种加标水平(5、10、100、1000μg/ kg)下噻虫啉的平均回收率在78.8%和107.1%之间,相对标准偏差(RSD)低于12.2%,定量限(LOQ)为5微克/千克。与报告的方法相比,该方法可以显着提高分析效率2到12倍,并减少5%至95%的溶剂消耗。用于研究噻虫啉在不同施用方式下在温室蔬菜和土壤中的消散率。噻虫啉在黄瓜和土壤中的半衰期为9.55–20.44天和3.74–9。在不同的施用方式下分别需要14天,在叶面喷洒的番茄中需要10.60天。根系灌溉下蔬菜中的残留量均少于叶面喷洒下的蔬菜。研究结果可为农业生产中噻虫啉的风险评估提供有用的数据。

更新日期:2018-02-16
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