基于磁性多壁碳纳米管的磁性固相萃取-超高效液相色谱-串联质谱法测定农产品中22种真菌毒素  

Magnetic Multi-Walled Carbon Nanotubes Nanomaterials as Magnetic Solid Phase Extraction Adsorbents for Simultaneous Determination of Multiple Mycotoxins in Agricultural Products by Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry

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作  者:马帅 梁刚[1] 满燕[1] 靳欣欣[1] 李安[1] MA Shuai;LIANG Gang;MAN Yan;JIN Xin-Xin;LI An(Institute of Quality Standard and Testing Technology of Beijing Academy of Agriculture and Forestry Sciences,Beijing 100097,China)

机构地区:[1]北京市农林科学院质量标准与检测技术研究所,北京100097

出  处:《分析化学》2024年第4期550-558,共9页Chinese Journal of Analytical Chemistry

基  金:国家自然科学基金项目(No.32202203);北京市农林科学院青年科研基金项目(No.QNJJ202245)资助。

摘  要:以磁性多壁碳纳米管(Fe_(3)O_(4)-MWCNTs)为吸附剂,建立了简单、快速和高效的磁性固相萃取方法,结合超高效液相色谱-串联质谱实现了对农产品中22种真菌毒素的同时检测。将Fe_(3)O_(4)纳米颗粒引入MWCNTs中制备Fe_(3)O_(4)-MWCNTs作为吸附剂,不仅可以提高多种目标真菌毒素的富集效率,还可通过外磁场进行分离,有效缩短了样品前处理时间。对影响磁性固相萃取前处理效率的提取溶液、吸附剂类型、吸附剂用量和洗脱溶液类型进行了优化。在最佳前处理条件下,结合超高效液相色谱-串联质谱进行检测,结果表明,22种真菌毒素在各自的浓度范围内均具有良好的线性关系(R2≥0.9966),方法检出限(LOD,S/N=3)为0.0008~1.6337 ng/g,定量限(LOQ,S/N=10)为0.0025~5.4457 ng/g,低、中、高3个浓度水平的加标回收率为71.5%~118.4%,日内精密度为1.3%~10.9%(n=6),日间精密度为2.3%~11.6%(n=3)。本方法前处理过程简单快速、有机溶剂消耗少、基质净化效率高,并且方法的线性范围宽、准确度和灵敏度高,可用于大批量农产品中多种真菌毒素的同时检测,对于保障粮食安全具有重要意义。A simple,rapid and efficient magnetic solid-phase extraction(MSPE) method was established by employing magnetic multi-walled carbon nanotubes(Fe_3O_4-MWCNTs) as adsorbents.And further,by coupling with ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS),an accurate quantitative approach for analysis of 22 kinds of mycotoxins in agricultural products was developed.With Fe_3O_4-MWCNTs as MSPE adsorbents,the enrichment efficiency of various target fungal toxins was improved and the sample pretreatment time was reduced effectively.In the pre-treatment stage,the extraction solution,adsorbent type,adsorbent dosage and elution solution type were systematically optimized.Under the optimal pre-treatment conditions of MSPE,the methodological investigation of the method was carried out.Under the optimal conditions,the proposed method showed a good linearity(R~2≥0.9966),high sensitivity(The limits of detection(S/N=3) were 0.0008–1.6337 ng/g and the limits of quantification(S/N=10) were 0.0025–5.4457 ng/g),adequate recoveries(71.5%–118.4%),and good repeatability(Intra-day precision in the range of 1.3%–10.9% and inter-day precision in the range of 2.3%–11.6%).The improved MSPE-UPLC-MS/MS analytical method had advantages inculding simplicity,rapidity and high efficiency,and could realize simultaneous detection of multiple mycotoxins in large quantities of agricultural products.

关 键 词:真菌毒素 磁性多壁碳纳米管 磁性固相萃取 超高效液相色谱-串联质谱 

分 类 号:O657.63[理学—分析化学] TS207.5[理学—化学]

 

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