Simultaneous determination of five pesticides residues in Anoectochilus roxburghii by HPLC-MS/MS method

Q4 Health Professions 药学服务与研究 Pub Date : 2020-10-31 DOI:10.5428/PCAR20200506
L. Wu, Mingke Luo, Wensheng He, Wenting Chen
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Abstract

Objective: To establish a HPLC-MS/MS method for simultaneous determination of five pesticides residues including tebuconazole,metalaxyl-M,thiophanate-methyl,oxytetracycline and abamectin in Anoectochilus roxburghii.Methods: The samples were extracted by acetonitrile solution and purified by QuEChERS method.Separation was performed on Agilent Eclipse Plus C18 column(50 mm×2.1 mm,1.8 μm) with the mobile phase consisting of 0.1% formic acid(A) and acetonitrile(B) by gradient elution(0-1.0 min,90% A;1.0-3.0 min,90%-70% A;3.0-5.0 min,70%-30% A;5.0-8.0 min,30%-10% A;8.0-14.0 min,10% A;14.0-15.0 min,10%-90% A;15.0-17.0 min,90% A).Detection was performed on a triple quadrupole tandem mass spectrometry with electrospray ionization source operating in positive ion mode under multiple reaction monitoring(MRM) mode.Results: The calibration curves of five pesticides showed good linearity coefficients(r>0.99).The average recoveries ranged from 72.7% to 94.9%(n=6),and the relative standard derivations(RSDs) were within 1.8%-10.3%(n=6).The detection limits of tebuconazole,metalaxyl-M,thiophanate-methyl,oxytetracycline and abamectin were 0.6,0.2,0.3,0.2,5.0 μg/kg,and the quantitation limits of 5 pesticides were 2.0,0.5,1.0,0.6 and 10.0 μg/kg respectively.Conclusion: The established method was proved to be sensitive,simple and reliable,and could be applied for the determination of these five pesticides in Anoectochilus roxburghii and quality control in the planting process.
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HPLC-MS/MS法同时测定金线莲中5种农药残留
目的:建立同时测定金线莲中戊唑醇、甲霜灵-M、甲基托布津、土霉素和阿维菌素5种农药残留量的HPLC-MS/MS方法。方法:样品用乙腈溶液提取,用QuEChERS法纯化。在Agilent Eclipse Plus C18柱(50 mm×2.1 mm,1.8μm)上进行分离,流动相由0.1%甲酸(A)和乙腈(B)组成,梯度洗脱(0-1.0分钟,90%A;1.0-3.0分钟,90%-70%A;3.0-5.0分钟,70%-30%A;5.0-8.0分钟,30%-10%A;8.0-14.0分钟,10%A;14.0-15.0分钟,10%-90%A;15.0-17.0分钟,90%A)在多重反应监测(MRM)模式下以正离子模式操作的具有电喷雾电离源的四极串联质谱法。结果:5种农药的线性关系良好(r>0.99),平均回收率为72.7%~94.9%(n=6),相对标准偏差在1.8%~10.3%(n=65种农药的定量限分别为2.0、0.5、1.0、0.6和10.0μg/kg。结论:建立的方法灵敏、简便、可靠,可用于金线莲中这5种农药的含量测定和种植过程中的质量控制。
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药学服务与研究
药学服务与研究 Health Professions-Pharmacy
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