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

Q4 Health Professions
L. Wu, Mingke Luo, Wensheng He, Wenting Chen
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引用次数: 0

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.
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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来源期刊
药学服务与研究
药学服务与研究 Health Professions-Pharmacy
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