多壁碳纳米管分散固相萃取净化超高效液相色谱串联质谱测定果蔬中50种农药残留量

Determination of 50 pesticide residues in fruits and vegetables by QuEChERS extraction with multi-walled carbon nanotubes (MWCNTs) coupled to UPLC-MS/MS

该文建立了以多壁碳纳米管(multi-walled carbon nanotube,MWCNT)结合Qu ECh ERS样品净化、超高效液相色谱串联质谱(ultra-performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)快速检测果蔬中50种农药残留物的分析方法,MWCNTs因其独特的中空结构和大比表面积而具有优异的吸附性能,使得它在果蔬农药残留分析的样品前处理过程中表现出优越的净化功效。通过优化实验,选择并确定了MWCNTs的型号和使用量,在Qu ECh ERS方法基础上改善了样品净化效果。果蔬样品用0.1%甲酸乙腈溶液提取,UPLCMS/MS对果蔬中50种农药残留物进行测定。结果表明,50种化合物的方法定量限为0.002~0.010 mg/kg;在线性范围内低、中、高3个添加水平的回收率为71%~105%,相对标准偏差为3.1%~11.2%。使用基质匹配标准曲线进行定量50种农药线性关系良好(r>0.99)。该方法具有简单、快速、灵敏度高、准确度高等优点,适合果蔬样品中农药多残留的快速检测分析。

This study intended to develop a method for the determination of 50 pesticide residues in fruits and vegetables by sample purification with QuEChERS of combing multi-walled carbon nanotube and ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). Because of its unique hollow structure and large specific surface area, multi-walled carbon nanotube has excellent adsorption properties, which make it shows superior purification efficiency in the sample pre-treatment process of pesticide residue analysis of fruits and vegetables. This paper selected and determined the type and usage of multi-walled carbon nanotubes through optimization experiments. Based on the QuEChERS method, this paper improved the sample purification effect. This paper extracted fruit and vegetable samples with 0.1% formic acid acetonitrile solution. Meanwhile, this paper detected 50 pesticide residues in fruits and vegetables through ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). The results demonstrated that they were 0.002-0.010 mg/kg for the limits of quantification(LOQs) for 50 compounds, 71%-105% recoveries of low, medium and high supplemental levels within the linear range and 3.1%-11.2% relative standard deviation(RSD). Good linearity of the Matrix matching standard curve was observed for all calibration curves with correlation coefficients(r) > 0.99. This method was rapid, high sensitivity and accuracy. It is suitable for rapid detection and analysis of pesticide residues in fruit and vegetable samples.