Oellig Claudia
Institute of Food Chemistry, University of Hohenheim , Garbenstrasse 28, 70599 Stuttgart, Germany.
J Agric Food Chem. 2016 Nov 2;64(43):8246-8253. doi: 10.1021/acs.jafc.6b03841. Epub 2016 Oct 19.
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.
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。