基于碳纳米材料改进QuEChERS结合GC-MS/MS检测茶叶中31种农药残留
Improved QuEChERS Method with Carbon Nanomaterials Combined with GC-MS/MS for the Detection of 31 Pesticide Residues in Tea Leaves
黄力群1
作者信息
- 1. 福建省产品质量检验研究院,福建 福州 350002
- 折叠
摘要
[目的]建立一种基于碳纳米材料改良分散固相萃取技术(QuEChERS)提高净化效果,并结合气相色谱-三重四级杆串联质谱法(GC-MS/MS)同时测定茶叶中 31种农药残留的检测方法.[方法]茶叶样品粉碎均匀后,利用碳纳米管作为吸附净化填料改良QuEChERS法净化,运用全自动QuEChERS样品前处理系统提取茶叶中的农药残留,用GC-MS/MS外标法定量.并比较了单壁碳纳米管(SWCNTs)、多壁碳纳米管(MWCNTs)以及氨基化多壁碳纳米管(MWCNTs-NH2)3种净化填料以及其在不同使用量情况下的净化效果.[结果]选用氨基化多壁碳纳米管(MWCNTs-NH2)改进传统QuEChERS填料,建立的GC-MS/MS检测方法检出限为0.02～1.68 μg·kg-1,定量限为 0.05～5.61 μg·kg-1;在低、中、高 3个水平加标回收率实验中,目标化合物的平均回收率为 81.0%～119.7%;相对标准偏差为 1.1%～10.0%.31种目标农药在茶叶中均表现出不同程度的基质效应,氯苯甲醚等 4种目标农药表现为基质抑制效应,而乐果等 27种目标农药表现为基质增强效应.[结论]该方法自动高效,灵敏度高,全过程耗时少,能有效的节省人力成本,适用于较大批量的茶叶样品检测.
Abstract
[Objective]A detection method based on modified dispersive solid-phase extraction with carbon nanomaterials(QuEChERS)to improve the cleanup effect and combined with gas chromatography-triple quadrupole tandem mass spectrometry(GC-MS/MS)for the simultaneous determination of 31 pesticide residues in tea was developed.[Method]The tea samples were pulverized uniformly and purified by the modified QuEChERS method using carbon nanotubes as adsorption and purification fillers,and the pesticide residues in tea were extracted using a fully automated QuEChERS sample pretreatment system and quantified by GC-MS/MS external standard method.The purification effects of three types of single-walled carbon nanotubes(SWCNTs),multi-walled carbon nanotubes(MWCNTs)and aminated multi-walled carbon nanotubes(MWCNTs-NH2)were compared with each other and in different amounts.[Result]In this study,aminated multi-walled carbon nanotubes(MWCNTs-NH2)were finally selected to improve the traditional QuEChERS filler,and the limits of detection(LODs)of this research method were 0.02～1.68 μg·kg-1,and the limits of quantification(LOQs)were 0.05～5.61 μg·kg-1;The average recoveries of the target compounds at the three levels of spiked recoveries,low,medium and high,were 81.0%～119.7%with the relative standard deviation(RSD)ranging from 1.1%to 10.0%.The target pesticides showed different degrees of matrix effects in tea,and four target pesticides,such as chloroanisole,showed matrix inhibitory effects,while 27 target pesticides,such as lecithromycin,showed matrix-enhancing effects.[Conclusion]The method is automatic and efficient,with high sensitivity,the whole process consumes less time,can effectively save labor costs,and is suitable for the detection of larger batches of tea samples.
关键词
碳纳米管/QuEChERS/农药残留/净化/茶叶/气相色谱-三重四级杆串联质谱Key words
Nanocarbon tubes/QuEChERS/pesticide residues/purification/tea/gas chromatography-triple quadrupole tandem mass spectrometry引用本文复制引用
出版年
2024
国家科技期刊平台
NSTL
万方数据