Martín-Calero Aurora, Ayala Juan H, González Venerando, Afonso Ana M
Department of Analytical Chemistry, Nutrition and Food Science, University of La Laguna, Campus de Anchieta, Astrofísico Francisco Sánchez s/n, E-38205 La Laguna, Spain.
Anal Chim Acta. 2007 Jan 23;582(2):259-66. doi: 10.1016/j.aca.2006.09.024. Epub 2006 Sep 19.
A procedure for the determination of less polar heterocyclic amines in meat extracts using solid phase microextraction (SPME) coupled to high-performance liquid chromatography (HPLC) with fluorescence detection is presented. Analytes were first extracted from the samples using methanol/NaOH by an ultrasound-assisted method, and then concentrated on a Carbowax-templated resin (CW-TPR) SPME fiber. The extraction conditions such as extractant mixture composition, extraction time and extractions number, were optimized and the need of an extract freezing step previous to SPME is discussed. The detection limits under optimal conditions are in the range of 0.28-1.1 ng g(-1). The method was applied to the determination of less polar heterocyclic amines in four commercial meat extracts. Recovery values obtained are higher than 60% for the majority of amines.
本文介绍了一种使用固相微萃取(SPME)与高效液相色谱(HPLC)联用荧光检测法测定肉类提取物中极性较小的杂环胺的方法。首先通过超声辅助法用甲醇/氢氧化钠从样品中提取分析物,然后将其浓缩在聚乙二醇模板树脂(CW-TPR)固相微萃取纤维上。优化了萃取剂混合物组成、萃取时间和萃取次数等萃取条件,并讨论了在固相微萃取之前进行提取物冷冻步骤的必要性。最佳条件下的检测限在0.28 - 1.1 ng g⁻¹范围内。该方法应用于四种市售肉类提取物中极性较小的杂环胺的测定。大多数胺类的回收率高于60%。