Li Runan, Chen Zenglong, Dong Fengshou, Xu Jun, Liu Xingang, Wu Xiaohu, Pan Xinglu, Tao Yan, Zheng Yongquan
State Key Laboratory for Biology of Plant Diseases and Insect Pests, Institute of Plant Protection, Chinese Academy of Agricultural Sciences, Beijing, 100193, PR China.
State Key Laboratory of Integrated Management of Pest Insects and Rodents, Institute of Zoology, Chinese Academy of Sciences, Beijing 100101, PR China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2018 Apr 1;1081-1082:25-32. doi: 10.1016/j.jchromb.2018.02.021. Epub 2018 Feb 16.
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 (UPC) BEH column (100 mm × 3.0 mm, 1.7 μm particle size) and thiacloprid was eluted at 1.22 min in gradient mode with CO/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.
首次开发了一种快速、灵敏且有效的超临界流体色谱-串联质谱(SFC-MS/MS)方法来分析噻虫啉。采用超高效汇聚色谱(UPC)BEH柱(100 mm × 3.0 mm,粒径1.7 μm)对SFC-MS/MS条件进行了优化,以CO/甲醇为流动相,在梯度模式下,噻虫啉在1.22 min时被洗脱。使用甲醇中0.1%的甲酸(v/v)作为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。噻虫啉在土壤中四个加标水平(5、10、100、1000 μg/kg)下的平均回收率在78.8%至107.1%之间,相对标准偏差(RSDs)低于12.2%,定量限(LOQ)为5 μg/kg。与已报道的方法相比,该方法可显著提高分析效率2至12倍,并减少溶剂消耗5%至95%。该方法用于研究不同施药模式下温室蔬菜和土壤中噻虫啉的消解速率。在不同施药模式下,噻虫啉在黄瓜和土壤中的半衰期分别为9.55至20.44天和3.74至9.14天,叶面喷施时在番茄中的半衰期为10.60天。根灌处理下蔬菜中的残留量均低于叶面喷施处理。该结果可为噻虫啉在农业生产中的风险评估提供有用数据。