二氯喹啉酸及其代谢物残留的QuEChERS-UHPLC/MS/MS分析及其室内消解动态研究
Studies on Simultaneous Analysis of Residues and Dissipation Dynamics of Quinclorac and Its Metabolites in Soil by QuEChERS-UHPLC-MS/MS
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摘要: 建立二氯喹啉酸及其代谢物二氯喹啉酸甲酯残留的QuEChERS-UHPLC-MS/MS （ultra performance liquid chromatography tandem mass spectrometry）分析方法，并研究室内培养条件下二氯喹啉酸的消解动态。样品经1%乙酸乙腈提取，C18净化剂净化，C18色谱柱分离，电喷雾离子源（ESI+），多反应监测（MRM）模式下分析。结果表明，二氯喹啉酸及其代谢物溶剂标准曲线和基质标准曲线在1.5~1 500 ng·mL-1范围内线性良好，回归分析可决系数（R2）为0.9993~1.0000。在0.001、0.03、0.3和3.0 mg·kg-1添加浓度下，二氯喹啉酸及二氯喹啉酸甲酯的平均添加回收率为78.20%~110.58%，相对标准偏差为1.43%~8.98%。二氯喹啉酸及其代谢物二氯喹啉酸甲酯测定方法的定量限为0.001 mg·kg-1；在温度25℃、60%湿度的室内条件下，初始加入量为0.3 mg·kg-1时旱地土二氯喹啉酸的半衰期为256.9 d，水稻土的半衰期为96.9 d；初始加入量为3.0 mg·kg-1时旱地土的半衰期为702.8 d，水稻土的半衰期为113.2 d。水稻土中60 d后才有二氯喹啉酸甲酯生成，旱地土中7 d后就有二氯喹啉酸甲酯生成。该方法简单、灵敏、准确、快速，能满足检测二氯喹啉酸及其代谢物在土壤中残留的要求。明确二氯喹啉酸的降解情况为二氯喹啉酸的生态风险评价和二氯喹啉酸的合理使用提供科学依据。Abstract: A method for the simultaneous determination of quinclorac and its metabolites in soil by ultra-performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) was established and the dissipation dynamics of quinclorac under lab conditions was investigated. The samples were extracted by acetonitrile containing 1% acetic acid and cleaned up by C18. The analytes were separated on a C18 column (50 mm×2.1 mm, 1.8 μm) and quantified by UHPLC/MS/MS system with selective ion quantitative determination in positive ion mode. The results showed that this method has good linearity in the range of 0.25~1 500 ng·mL-1 under the optimized analysis conditions with coefficient of determination (R2) of 0.9993~1.0000. At the spiked concentration of 0.001, 0.03, 0.3, 3.0 mg·kg-1, the recoveries of quinclorac and its metabolites in soil were ranged from 78.20% to 110.58%, with relative standard deviation (RSD) of 1.43%~8.98%. The limit of quantification (LOQ) of this method was 0.001 mg·kg-1. At the initial spiked concentration of 0.3 mg·kg-1, the dissipation half-lives of quinclorac in dryland soil and paddy soil was 256.9 d and 96.9 d respectively; however, at 3.0 mg·kg-1 spiked concentration, the half-lives of quinclorac in dryland soil and paddy soil was increased to 702.8 d and 113.2 d. Quinclorac methyl ester was formed in paddy soil after 60 d and quinclorac methyl ester was formed in dry soil after 7 d of incubation. The developed method is simple, sensitive, accurate and rapid, and could meet the requirement of residue detection of quinclorac and its metabolites in soil. Evaluating the fate of quinclorac and its metabolites quinclorac methyl ester in soil is important in residue control, environmental risk assessment and the rational use of this herbicide.
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