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气相色谱串联质谱法中通过引入保留间隙提高红辣椒粉农药残留定量分析的色谱性能

Improved chromatographic performance in red chilli powder pesticide residue quantitation by retention gap introduction in gas chromatography tandem mass spectrometry.

作者信息

Kandaswamy Chandrasekar, Presley Davis, Ahammed T P Shabeer, Anadaram Sreekanth

机构信息

Agilent Technologies, Bangalore, India.

Department of Chemistry, Sri Sivasubramaniya Nadar College of Engineering, Chennai, 603110 India.

出版信息

J Food Sci Technol. 2022 May;59(5):1692-1703. doi: 10.1007/s13197-021-05177-3. Epub 2021 Jul 5.

Abstract

UNLABELLED

Analysis of agrochemical residues in red chilli powder is always considered difficult because of higher matrix interference due to carotenoid pigments and other co-extractives. During the sample preparation, matrix components were co-extracted along with the target compounds leading to frequent source cleaning, changing of liner and column. Efforts were made to improve the chromatographic performance by optimizing sample preparation, choosing matrix-free transitions and introducing a retention gap. The Quick, Easy, Cheap, Effective, Rugged and Safe (QuEChERS) extraction was experimented using different dispersive adsorbents and the purified extract was analyzed by gas chromatography tandem mass spectrometry (GC-MS/MS) system. 84 pesticides under different class were validated and established a limit of quantification of 0.002-0.007 mgkg. The recovery was between 70 and 110% at 0.01, 0.025 and 0.05 mgkg fortification level and corresponding precision was between 3 and 16% RSD. Suitability of the validated method was established through analysis of market samples of chilli powder for the quantitation of targeted pesticide residues.

SUPPLEMENTARY INFORMATION

The online version contains supplementary material available at 10.1007/s13197-021-05177-3.

摘要

未标记

由于辣椒粉中类胡萝卜素色素和其他共提取物造成的较高基质干扰,对辣椒粉中农药残留的分析一直被认为很困难。在样品制备过程中,基质成分与目标化合物一起被共提取,导致频繁进行进样口清洗、更换衬管和色谱柱。通过优化样品制备、选择无基质的跃迁和引入保留间隙,努力提高色谱性能。使用不同的分散吸附剂对快速、简便、廉价、高效、耐用和安全(QuEChERS)萃取法进行了实验,并通过气相色谱串联质谱(GC-MS/MS)系统对纯化后的提取物进行分析。对84种不同类别的农药进行了验证,确定定量限为0.002 - 0.007 mg/kg。在0.01、0.025和0.05 mg/kg的加标水平下,回收率在70%至110%之间,相应的精密度为3%至16%相对标准偏差。通过分析辣椒粉市场样品中目标农药残留的定量,确定了验证方法的适用性。

补充信息

在线版本包含可在10.1007/s13197-021-05177-3获取的补充材料。

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