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| 超高效液相色谱串联质谱检测啶菌噁唑等6种农药在我国典型土壤中的残留 |
| Simultaneous determination of pyrisoxazole and five other pesticides in typical types of Chinese soil using ultra-performance liquid chromatography and tandem mass spectrometry |
| Received:November 28, 2019 |
| DOI：10.13254/j.jare.2019.0581 |
| 中文关键词: UPLC-MS/MS，土壤，农药，QuEChERS，残留检测 |
| 英文关键词: UPLC-MS/MS, soil, pesticide, QuEChERS, residue analysis |
| 基金项目:中国农业科学院科技创新工程协同创新任务（CAAS-XTCX2016015） |
| Author Name | Affiliation | E-mail | | JIAO Bin | Institute of Plant Protection, Chinese Academy of Agricultural Sciences, Beijing 100193, China | | | XU Jun | Institute of Plant Protection, Chinese Academy of Agricultural Sciences, Beijing 100193, China | junxu1@ippcaas.cn | | LIU Xin-gang | Institute of Plant Protection, Chinese Academy of Agricultural Sciences, Beijing 100193, China | | | DONG Feng-shou | Institute of Plant Protection, Chinese Academy of Agricultural Sciences, Beijing 100193, China | | | WU Xiao-hu | Institute of Plant Protection, Chinese Academy of Agricultural Sciences, Beijing 100193, China | | | ZHENG Yong-quan | Institute of Plant Protection, Chinese Academy of Agricultural Sciences, Beijing 100193, China | |
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| 中文摘要: |
| 为了建立啶菌噁唑、氯噻啉、呋喃虫酰肼、丁吡吗啉、丁香菌酯和毒氟磷在我国典型土壤中的残留检测方法，采用QuEChERS方法进行样品前处理，优化提取溶剂及净化剂，应用超高效液相色谱串联质谱（UPLC-MS/MS）进行质谱及液相方法的开发并进行样品检测。结果表明：乙腈作为提取溶剂，提取物颜色较浅，干扰物含量较低；佛罗里硅土结合石墨化炭黑作为净化剂净化效果较理想。在0.5~50 mg·L-1范围内，6种农药的进样质量浓度与对应的峰面积间呈良好的线性关系，R2>0.990 0，定量限均为1 mg·kg-1。在1、10、100 mg·kg-1 3个添加水平下，平均回收率为73.3%~117.2%，相对标准偏差均小于17.3%。研究表明，本研究建立的分析方法在准确度、灵敏度和精密度上均满足残留分析要求，可以为啶菌噁唑、氯噻啉、呋喃虫酰肼、丁吡吗啉、丁香菌酯和毒氟磷在我国典型土壤中的残留检测提供方法支撑。 |
| 英文摘要: |
| In order to establish a method for determining pyrisoxazole, imidaclothiz, fufenozide, pyrimorph, coumoxystrobin, and dufulin intypical Chinese soils, we conducted an experiment using a quick, easy, cheap, effective, rugged, and safe(QuEChERS)method and ultraperformance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). Extraction solvents, purification adsorbents, mass detection, and chromatographic separation conditions were all optimized. Acetonitrile was selected as an extraction solvent, as the extracts obtained were lighter in color and contained a fewer impurities, whereas florisil and graphitized carbon black were selected as purification adsorbents based on their excellent performance. The method showed excellent linearity(R2>0.990 0)in the range of 0.5 to 50 mg·L-1, and the limit of quantification for all six compounds in soil was 1 mg·kg-1. The mean recoveries from soil for the six target compounds at fortification levels of 1, 10, and 100 mg·kg-1 ranged from 73.3% to 117.2%, with relative standard deviations lower than 17.3%. The method established in this study meets the requirements of residue analysis in terms of accuracy, sensitivity, and precision, and can thus be applied to monitor pyrisoxazole, imidaclothiz, fufenozide, pyrimorph, coumoxystrobin, and dufulin residues in soil samples. |
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