QuEChERS-UPLC-MS/MS法快速筛查稻米和稻茎中42种农药残留 |
投稿时间:2019-05-06
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引用本文:李亚辉,姚春霞,周佳欣,等.QuEChERS-UPLC-MS/MS法快速筛查稻米和稻茎中42种农药残留[J].农药学学报,2019,21(4):483-491. |
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基金项目:沪农科推字(2018)第1-5号;上海市科委项目(17712400800,16391900500);上海市崇明区科委攻关项目(CKS2018-12) |
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中文摘要:建立了QuEChERS前处理技术结合超高效液相色谱-串联质谱(UPLC-MS/MS)同时检测稻米和稻茎中42种农药残留的分析方法。样品经乙腈涡旋提取、QuEChERS净化管净化,C18超高效液相色谱柱分离后,在电喷雾正离子(ESI+)模式下,通过多反应监测正离子模式进行检测,采用基质匹配标准曲线峰面积外标法进行定量分析。结果表明:在0.01~0.2 mg/L范围内,42种农药的质量浓度与对应的峰面积间线性关系良好,R2 > 0.99,检出限为0.001~0.002 mg/kg。在0.01、0.02、0.05、0.1和0.2 mg/kg 5个添加水平下,42种农药在稻米和稻茎中的平均回收率均为70%~117%,相对标准偏差(RSD)稻米为1.5%~15%和稻茎为0.9%~15%。该方法具有操作简单、快速、灵敏度高、准确度高等优点,适用于稻米和稻茎中多种类农药残留的快速筛查分析。 |
中文关键词:QuEChERS 超高效液相色谱-串联质谱 稻米 稻茎 农药多残留 甲胺磷 甲霜灵 丙草胺 |
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Rapid screening of 42 pesticides in rice and rice stems by QuEChERS-UPLC-MS/MS |
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Abstract:A method for the analysis of 42 pesticide residues in rice and rice stems was developed using ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) combined with QuEChERS pretreatment technology. The sample was extracted with acetonitrile vortex extraction, purified by QuEChERS purification tube and separated by C18 ultra-high performance liquid chromatography column. 42 analytes were measured under multiple reaction monitoring (MRM) using the electrospray positive ionization mode (ESI+). Quantification determination was performed by peak area external standard methods using matrix-matched calibration, which were linear in the range of 0.01-0.2 mg/L with good linear relationships. The determination coefficients (R2) were all above 0.99. The limits of detection (LOD) were lower than 0.002 mg/kg. The average recoveries of 42 pesticides in rice and rice stems all ranged from 70%-117%, and the relative standard deviations were in the range of 1.5%-15% in rice, and 0.9%-15% in rice stems, at the spiked levels of 0.01, 0.02, 0.05, 0.1 and 0.2 mg/kg. This method is simple, rapid, sensitivite, accuracy, which can be used in the simple and rapid screening of pesticide multi-residues in rice and rice stems. |
Key words:QuEChERS ultra performance liquid chromatography-tandem mass spectrometry rice rice stems multi-residues of pesticides methamidophos metalaxyl pretilachlor |
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