超高效液相色谱-串联质谱法测定浙贝母中6种农药残留
投稿时间：2018-02-11      点此下载全文 HTML
引用本文：俞建忠,苍涛,戴芬,等.超高效液相色谱-串联质谱法测定浙贝母中6种农药残留[J].农药学学报,2018,20(3):370-376.
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俞建忠 省部共建国家重点实验室培育基地——浙江省植物有害生物防控重点实验室, 农业部农药残留检测重点实验室, 浙江省农业科学院 农产品质量标准研究所, 杭州 310021  
苍涛 省部共建国家重点实验室培育基地——浙江省植物有害生物防控重点实验室, 农业部农药残留检测重点实验室, 浙江省农业科学院 农产品质量标准研究所, 杭州 310021  
戴芬 省部共建国家重点实验室培育基地——浙江省植物有害生物防控重点实验室, 农业部农药残留检测重点实验室, 浙江省农业科学院 农产品质量标准研究所, 杭州 310021  
赵学平 省部共建国家重点实验室培育基地——浙江省植物有害生物防控重点实验室, 农业部农药残留检测重点实验室, 浙江省农业科学院 农产品质量标准研究所, 杭州 310021 zhaoxueping@tom.com 
基金项目:国家自然科学青年基金（31501685）；浙贝母全产业链质量安全风险管控（ZJNY2017001-05）
中文摘要:建立了QuEChERS-超高效液相色谱-串联质谱（UPLC-MS/MS）同时测定浙贝母鲜样和干样中吡虫啉、啶菌唑、氟唑菌酰胺、嘧菌环胺、吡唑醚菌酯和阿维菌素共6种农药残留量的方法。样品用V（乙腈）：V（水）=4：1混合溶液提取，经C18 50 mg+PSA 50 mg+MgSO4 150 mg净化，采用UPLC-MS/MS电喷雾离子化正离子扫描和多反应监测模式（MRM）测定，基质匹配标准溶液外标法定量。结果表明：在0.001~0.2 mg/L范围内，6种农药的质量浓度与相应的峰面积间呈良好的线性关系，相关系数均大于0.994。6种农药在浙贝母鲜样中的定量限（LOQ）为0.01 mg/kg，检出限（LOD）为2×10–5~3×10–4 mg/kg，在干样中的LOQ为0.05 mg/kg，LOD为1×10–4~1×10–3 mg/kg。在0.01、0.5和2 mg/kg添加水平下，6种农药在浙贝母鲜样中的平均回收率均在80%~109%之间，相对标准偏差（RSD）在0.95%~13%之间（n=5）；在0.05、0.5和2 mg/kg添加水平下，6种农药在浙贝母干样中的平均回收率均在77%~101%之间，RSD在0.89%~7.5%之间（n=5）。经实际样品检测验证，该方法快速、简便、可靠、高效，适用于同时检测浙贝母中吡虫啉、啶菌唑、氟唑菌酰胺、嘧菌环胺、吡唑醚菌酯和阿维菌素等农药的残留。
中文关键词:超高效液相色谱-串联质谱(UPLC-MS/MS)  浙贝母  QuEChERS  农药  残留
 
Determination of 6 pesticides residues in Fritillaria thunbergii by ultra performance liquid chromatography-tandem mass spectrometry
Abstract:A method for the simultaneous determination of imidacloprid, pyrisoxazole, fluxapyroxad, cyprodinil, pyraclostrobin, abamectin in Fritillaria thunbergii Miq. was developed using QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). F. thunbergii samples were extracted by V(acetonitrile):V(water)=4:1. Then they were cleaned up by PSA 50 mg + C18 50 mg + MgSO4150 mg adsorbents and detected by UPLC-MS/MS under positive polarity multiple reactions monitoring (MRM) mode. The matrix-matched external standard calibration curves were used for quantitative analysis. The linearities of 6 pesticides were all in the range of 0.001-0.2 mg/L, with correlation coefficients higher than 0.994. The limit of quantification (LOQ) was 0.01 mg/kg and the limits of detection (LOD) of this new method were 2×10-5 mg/kg to 3×10-4 mg/kg in fresh F. thunbergii. While the LOQ was 0.05 mg/kg and the LOD of the proposed method were 1×10-4 mg/kg to 1×10-3 mg/kg in dry F. thunbergii. Recoveries at three spiked levels of 0.01, 0.5 and 2 mg/kg ranged from 80% to 109% with relative standard deviations (RSDs) from 0.95% to 13% (n=5) in fresh F. thunbergii. While, in dry F. thunbergii, recoveries at three spiked levels of 0.05, 0.5 and 2 mg/kg ranged from 77% to 101% with RSDs from 0.89% to 7.5% (n=5). The application of this new method in real samples has been demonstrated. Given that this method is fast, simple, accurate and efficient, it can meet the requirements for the determination of residues of imidacloprid, pyrisoxazole, fluxapyroxad, cyprodinil, pyraclostrobine, abamectin in F. thunbergii.
Key words:ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)  Fritillaria thunbergii  QuEChERS  pesticide  residue
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