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、啶菌齅唑、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C1850 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、啶菌齅唑、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。
A method for the simultaneous determination of imidacloprid, pyrisoxazole, fluxapyroxad,cyprodinil, pyraclostrobin, abamectin in Fritillaria thunbergii Miq. was developed using Qu ECh ERSultra 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 ＋ MgSO4 150 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.
作者
俞建忠
苍涛
戴芬
赵学平
YU Jianzhong;CANG Tao;DAI Fen;ZHAO Xueping(State Key Laboratory Breeding Base for Zhejiang Sustainable Plant Pest Control, MOA Key Labroatoty for Pesticide Residue Detection Institute of QualiO, and Standard for Agro-Products, Zhejiang Academy of Agricultural Sciences, Hangzhou 310021, China)
出处
《农药学学报》
CAS
CSCD
北大核心
2018年第3期370-376,共7页
Chinese Journal of Pesticide Science
基金
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)
