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气相色谱结合过滤净化和固相萃取法测定水果、蔬菜和食用菌中多种农药残留的比较

A comparison of the determination of multiple pesticide residues in fruits, vegetables, and edible fungi using gas chromatography combined with filtration purification and solid-phase extraction.

作者信息

Zeng Yan, Lan Tao, Li Xiaxue, Chen Ya, Yang Qiaohui, Qu Bin, Zhang Yu, Pan Canping

机构信息

Ya'an Agricultural Food Quality Monitoring and Testing Center Ya'an 625000 China.

China National Institute of Standardization Beijing 100191 China.

出版信息

RSC Adv. 2024 May 24;14(24):16898-16911. doi: 10.1039/d3ra07584b. eCollection 2024 May 22.

Abstract

The multiplug filtration clean-up (m-PFC) and solid-phase extraction (SPE) pretreatment methods were employed to process 8 representative matrices in fruits, vegetables, and edible fungi, respectively. 37 pesticide residues were determined using gas chromatography equipped with ECD and FPD detectors. The measurement data were compared and analyzed following m-PFC purification and gas chromatography analysis, and both accuracy and precision met the (EU) 2021/808 requirements, achieving recovery rates for the 8 matrices ranging from 67.0% to 112.8% (averaging over 83.8% recovery), and RSDs between 0.2% and 15.2%. The 37 pesticides exhibited good linearity between 0.05 and 1.6 μg mL, and the matrix effect was found to be weaker compared to that of the Florisil solid-phase extraction method. The detection limits ranged from 0.0001 to 0.03 μg kg, with 31 pesticides showing lower detection limits compared to the SPE method. The application of this method to 150 real samples resulted in the detection of 17 pesticides across all samples. Fewer pigments were detected in m-PFC purified solutions compared to Florisil PR SPE when analyzed by liquid chromatography. m-PFC achieved more thorough adsorption of endogenous substances like pigments, reducing instrument contamination, utilizing less organic solvent, and simplifying the operation. This purification step offers clear advantages, allowing for the processing of larger sample batches in a short time. It can serve as a replacement for SPE methods like Florisi PR in batch detection of fruit and vegetable samples.

摘要

采用多插头过滤净化(m-PFC)和固相萃取(SPE)预处理方法分别对水果、蔬菜和食用菌中的8种代表性基质进行处理。使用配备电子捕获检测器(ECD)和火焰光度检测器(FPD)的气相色谱法测定37种农药残留。对m-PFC净化和气相色谱分析后的测量数据进行比较和分析,准确度和精密度均符合(欧盟)2021/808要求,8种基质的回收率在67.0%至112.8%之间(平均回收率超过83.8%),相对标准偏差(RSD)在0.2%至15.2%之间。37种农药在0.05至1.6 μg/mL之间呈现良好的线性关系,且与弗罗里硅土固相萃取法相比,基质效应较弱。检测限在0.0001至0.03 μg/kg之间,31种农药的检测限低于SPE法。将该方法应用于150个实际样品,所有样品中共检测出17种农药。液相色谱分析时,与弗罗里硅土PR SPE相比,m-PFC净化溶液中检测到的色素较少。m-PFC对色素等内源性物质的吸附更彻底,减少了仪器污染,并减少了有机溶剂的使用,简化了操作。这一净化步骤具有明显优势,能够在短时间内处理更大批量的样品。它可替代弗罗里硅PR等SPE方法用于果蔬样品的批量检测。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/48e8/11123614/5fbd7c32346f/d3ra07584b-f1.jpg

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