沈菁　王小飞　陈舒　陈思　彭西甜

摘要：采用QuEChERS的前处理方法，建立了一种简单、快速、灵敏的水稻糙米中吡唑醚菌酯残留量的超高效液相色谱-串联质谱（UPLC-MS/MS）分析方法。该方法以乙腈作为萃取溶剂，经液液分配萃取后，盐析分层，N-丙基-乙二胺键合硅胶（PSA）和C18键合硅胶净化后，进行超高效液相色谱-串联质谱（UPLC-MS/MS）分析，实现了样品的快速提取、净化、分离和检测。在优化条件下，吡唑醚菌酯在0.01～0.5 mg/L的范围内浓度与峰面积呈良好线性关系（R2=0.990 0），回收率为82%～106%，相对标准偏差小于11%，该方法具有较好的准确度和精密度。经水稻田间试验，发现糙米中的吡唑醚菌酯残留量在0.006～0.023 mg/kg之间。

关键词：吡唑醚菌酯；QuEChERS；超高效液相色谱-串联质谱（UPLC-MS/MS）；糙米；最终残留

中图分类号：O658 文献标识码：A 文章编号：0439-8114（2015）24-6366-03

DOI：10.14088/j.cnki.issn0439-8114.2015.24.070

Abstract：In this paper，a high efficient，rapid and sensitive determination method of pyraclostrobine in brown rice samples was proposed by a modified QuEChERS （quick，easy，cheap，effective，rugged and safe） method. Acetonitrile （ACN） was used to extract the residue of pyraclostrobine in samples.After salting out，the organic layer was cleaned up using PSA and C18 sorbents，and then the solution was directly analyzed by ultra-high-performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS），resulting in rapid extraction，clean-up，separation and detection of pyraclostrobine in samples. Under the optimized LC and MS conditions，good linearity in the range of 0.01～0.05 mg/kg was obtained for pyraclostrobine with R2 of 0.990 0.The method recoveries of the pyraclostrobine spiked at low，middle and high concentrations in blank rice samples were from 82% to 106%，with relative standard deviations less than 11%，indicating that the proposed method has good accuracy and precision.At last，the proposed method was applied to analyze the final residues of pyraclostrobine in samples，and the residues of pyraclostrobine in brown rice samples were in the range of 0.006～0.023 mg/kg.

Key words：pyraclostrobine；QuEChERS；utra-high-performance liquid chromatography-tandem mass spectrometry； brown rice；final residues

吡唑醚菌酯又名唑菌胺酯、百克敏，是一种含有吡唑结构的甲氧基丙烯酸酯类杀菌剂[1]，可以防治由多种真菌病原引起的病害，例如谷类作物的白粉病、锈病、叶枯病等[2，3]。目前，吡唑醚菌酯在农业生产中应用较为广泛，其在作物中的残留不可避免，因此开展作物中吡唑醚菌酯残留的检测方法研究很有必要。吴洁珊等[4]采用气相色谱测定柑橘中多种甲氧基丙烯酸酯类杀菌剂的残留量；薄海波等[5]采用气相色谱-质谱法测定食品中甲氧基丙烯酸酯类杀菌剂残留；徐英江等[6]采用液相色谱串联质谱测定蔬菜中残留的吡唑醚菌酯。传统的紫外或荧光检测器在低残留水平下抗干扰能力差，常常出现假阳性结果，而质谱检测器具有灵敏度高、选择性好等特点，可以实现复杂样品中农药残留的高灵敏度定性和定量分析，因此近年来在农药残留分析中应用非常广泛。……