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高效薄层色谱荧光检测法筛选蓖麻油酸作为黑麦角中黑麦的化学标志物

Screening for Ricinoleic Acid as a Chemical Marker for Secale cornutum in Rye by High-Performance Thin-Layer Chromatography with Fluorescence Detection.

作者信息

Oellig Claudia

机构信息

Institute of Food Chemistry, University of Hohenheim , Garbenstrasse 28, 70599 Stuttgart, Germany.

出版信息

J Agric Food Chem. 2016 Nov 2;64(43):8246-8253. doi: 10.1021/acs.jafc.6b03841. Epub 2016 Oct 19.

Abstract

Ricinoleic acid as the characteristic fatty acid of Secale cornutum oil is a good marker for Secale cornutum impurities in cereal. The presented screening for ricinoleic acid in rye by high-performance thin-layer chromatography with fluorescence detection (HPTLC-FLD) offers a selective and sensitive method for the determination of Secale cornutum and is very different from existing gas chromatographic analyses. Lipid extraction was followed by transesterification and solid-phase extraction cleanup; thereafter, extracts were selectively derivatized with 2-naphthoyl chloride and analyzed by HPTLC-FLD with silica gel plates and cyclohexane/diisopropyl ether/formic acid (86:14:1, v/v/v) as mobile phase. For quantitation, the enhanced fluorescence was scanned at 280/>340 nm. Limits of detection and quantitation of 0.1 and 0.4 mg ricinoleic acid/kg of rye were obtained, which enables the determination of Secale cornutum far below the maximum admitted level. With near-100% recoveries and low standard deviations at relevant spiking levels, reliable results were guaranteed.

摘要

蓖麻油酸作为黑麦角油的特征脂肪酸,是谷物中黑麦角杂质的良好标志物。本文介绍的采用荧光检测的高效薄层色谱法(HPTLC-FLD)对黑麦中的蓖麻油酸进行筛选,为黑麦角的测定提供了一种选择性和灵敏的方法,与现有的气相色谱分析方法有很大不同。脂质提取后进行酯交换和固相萃取净化;此后,提取物用2-萘甲酰氯进行选择性衍生化,并用硅胶板和环己烷/二异丙醚/甲酸(86:14:1,v/v/v)作为流动相进行HPTLC-FLD分析。为了定量,在280/>340nm处扫描增强荧光。获得了0.1和0.4mg蓖麻油酸/千克黑麦的检测限和定量限,这使得能够测定远低于最大允许水平的黑麦角。在相关加标水平下,回收率接近100%,标准偏差低,保证了可靠的结果。

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