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采用微波辅助提取-分散液-液微萃取法分析牛肉汉堡中的非极性杂环芳香胺。

Analysis of non-polar heterocyclic aromatic amines in beefburguers by using microwave-assisted extraction and dispersive liquid-ionic liquid microextraction.

机构信息

Laboratorio de Separaciones Analíticas, División Química Analítica, Facultad de Ciencias Exactas, Universidad Nacional de La Plata, 47 y 115, 1900 La Plata, Argentina.

出版信息

Food Chem. 2013 Dec 1;141(3):1694-701. doi: 10.1016/j.foodchem.2013.04.076. Epub 2013 May 2.

Abstract

A new sample preparation procedure to determine six heterocyclic aromatic amines (3-Amino-1,4-dimethyl-5H-pirido[4,3-b]indole, 3-Amino-1-methyl-5H-pirido[4,3-b]indole, 2-amino-1-methyl-6-phenylimidazo-[4,5-b]pyridine, 2-amino-9H-pyrido-[2,3-b] indole, 2-amino-3-methyl-9H-pyrido-[2,3-b] indole and 2-Amino-1,6-dimethylimidazo [4,5-b]-pyridine) in cooked beefburguers by using a combination of microwave-assisted solvent extraction and dispersive liquid-liquid microextraction with an ionic liquid generated in situ was used. The optimized microwave extraction procedure consisted of a clean-up step with n-heptane and a subsequent dissolution step in basic media to desorb the analytes from the matrix. Next, an aqueous solution of the ionic liquid 1-octyl-3-methylimidazolium tetrafluorborate and sodium hexafluorphosphate was added and a water-insoluble 1-octyl-3-methylimidazolium hexafluorphosphate was formed within the matrix sample. The amines were analyzed by liquid chromatography with fluorescence and diode-array detection by using a typical C18 column. Peak identities were confirmed by absorbance spectral matching. Repeatability (RSD%) between 5.4% and 10.9%, enrichment factors between 19 and 30, limits of detection between 0.35 and 2.4 ng mL(-1) and recoveries between 69% and 100% were achieved. The extraction methodology is simple, rapid (about 40 min/sample) cheap and green since small amounts of non-toxic solvents are necessary.

摘要

一种新的样品前处理方法,用于通过微波辅助溶剂萃取和分散液液微萃取相结合,原位生成离子液体,来测定熟牛肉汉堡中的六种杂环芳香胺(3-氨基-1,4-二甲基-5H-吡啶并[4,3-b]吲哚、3-氨基-1-甲基-5H-吡啶并[4,3-b]吲哚、2-氨基-1-甲基-6-苯基咪唑并[4,5-b]吡啶、2-氨基-9H-吡啶并[2,3-b]吲哚、2-氨基-3-甲基-9H-吡啶并[2,3-b]吲哚和 2-氨基-1,6-二甲基咪唑并[4,5-b]吡啶)。优化的微波萃取程序包括用正庚烷进行清洗步骤,然后在碱性介质中进行后续溶解步骤,以将分析物从基质中解吸出来。接下来,加入离子液体 1-辛基-3-甲基咪唑四氟硼酸盐和六氟磷酸钠的水溶液,并在基质样品内形成不溶于水的 1-辛基-3-甲基咪唑六氟磷酸盐。采用典型的 C18 柱,通过荧光和二极管阵列检测进行液相色谱分析。通过吸光度谱匹配确认峰的身份。重复性(RSD%)在 5.4%至 10.9%之间,富集因子在 19 至 30 之间,检测限在 0.35 至 2.4 ng mL(-1) 之间,回收率在 69%至 100%之间。该提取方法简单、快速(约 40 分钟/样品)、廉价且绿色,因为只需要少量无毒溶剂。

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