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胶束电动毛细管色谱法与反相液相色谱法测定咖喱中香豆素的含量

Sweeping-micellar electrokinetic chromatography versus reversed phase liquid chromatography for the determination of coumarin in curry.

机构信息

Australian Centre for Research on Separation Science, School of Natural Sciences-Chemistry, University of Tasmania, Hobart, Tasmania 7001, Australia.

Australian Centre for Research on Separation Science, School of Natural Sciences-Chemistry, University of Tasmania, Hobart, Tasmania 7001, Australia.

出版信息

J Chromatogr A. 2021 Nov 8;1657:462586. doi: 10.1016/j.chroma.2021.462586. Epub 2021 Oct 2.

Abstract

Coumarin is a phytotoxin found in the popular spice cinnamon, which is used to flavor many Asian curry dishes. In this work, we developed and compared the analytical performance of reversed-phase liquid chromatography (RP-LC) and sweeping-micellar electrokinetic chromatography (MEKC) methods for the determination of coumarin in complex curry (gravy) samples. Using a matrix matched sample (curry after solvent extraction with methanol and diluted with 100 mM phosphoric acid), the intra-day and inter-day repeatability of retention/migration time and (corrected) peak area for both methods were acceptable (%RSD (n=6) ≤ 5%). The linear range and limit of quantitation (LOQ) were an order of magnitude better in RP-LC (RP-LC linear range = 0.11-108 mg/kg, LOQ = 0.11 mg/kg) (Sweeping-MEKC linear range = 2.16-216 mg/kg, LOQ = 2.16 mg/kg). However, the limit of detection (S/N=3) and LOQ in sweeping-MEKC was 0.65 mg/kg and 2.16 mg/kg, which were sufficient to report the levels of coumarin ≥ the European limit of 2 mg/kg in foods. During the analysis of 25 curry samples, relatively similar results for sweeping-MEKC and RP-LC were obtained for 6 samples that contained coumarin >LOQ of sweeping-MEKC. Interferences in RP-LC lead to significant overestimation of coumarin levels in 3 samples. Coumarin levels above the EU limit was found in 6 curry samples using the more selective sweeping-MEKC. This work should also raise public awareness on the presence of potentially high levels of coumarin in some foods.

摘要

香豆素是一种存在于常见香料肉桂中的植物毒素,用于为许多亚洲咖喱菜肴调味。在这项工作中,我们开发并比较了反相液相色谱(RP-LC)和胶束电动色谱(MEKC)方法在复杂咖喱(肉汁)样品中测定香豆素的分析性能。使用基质匹配样品(用甲醇溶剂提取后与 100 mM 磷酸稀释的咖喱),两种方法的保留/迁移时间和(校正)峰面积的日内和日间重复性均可接受(%RSD(n=6)≤5%)。RP-LC 的线性范围和定量限(LOQ)高一个数量级(RP-LC 线性范围=0.11-108 mg/kg,LOQ=0.11 mg/kg)(Sweeping-MEKC 线性范围=2.16-216 mg/kg,LOQ=2.16 mg/kg)。然而,在 Sweeping-MEKC 中,检测限(S/N=3)和 LOQ 为 0.65 mg/kg 和 2.16 mg/kg,足以报告食品中香豆素水平≥2 mg/kg 的欧盟限量。在分析 25 个咖喱样品时,对于含有香豆素> Sweeping-MEKC LOQ 的 6 个样品,Sweeping-MEKC 和 RP-LC 得到了相对相似的结果。在 3 个样品中,RP-LC 中的干扰导致香豆素水平的显著高估。使用更具选择性的 Sweeping-MEKC 在 6 个咖喱样品中发现了香豆素含量超过欧盟限量的情况。这项工作还应引起公众对一些食品中存在潜在高含量香豆素的关注。

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