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比较用于测定炭烤肉和鱼中多环芳烃的色谱分析的提取程序和定量方法。

A comparison of the extraction procedures and quantification methods for the chromatographic determination of polycyclic aromatic hydrocarbons in charcoal grilled meat and fish.

机构信息

REQUIMTE, Laboratório de Bromatologia e Hidrologia, Departamento de Ciências Químicas, Faculdade de Farmácia da Universidade do Porto, Portugal.

出版信息

Talanta. 2012 Jan 15;88:677-83. doi: 10.1016/j.talanta.2011.11.060. Epub 2011 Nov 26.

Abstract

A method for analysis of 15 PAHs in charcoal-grilled meat/fish was established by high performance liquid chromatography and fluorescence detection. Gradient elution was performed with methanol/water/ethyl acetate. Maxima excitation and emission wavelengths were selected for each PAH. Retention times were very stable with coefficients of variation below 0.24% within analytical day and below 0.60% across analytical days. Two different methods of cleanup and pre-concentration steps were compared. Solvent extraction assisted by sonication carried out with n-hexane on 2g of lyophilized meat or 1g of lyophilized fish allowed to obtain high sensitivity, reproducibility and better extraction efficiency. Limits of quantification (LOQs, s/n=10) were lower than 0.01ng/g of meat wet weight and lower than 0.02ng/g of fish wet weight for all PAHs (except for Na, Fl and IP that were lower than 0.1ng/g). Two different quantification methods were compared. Standard addition method compensated PAHs losses due to incomplete extraction and it is recommended for analyses of grilled meat and fish samples that usually contain very low amounts of the eight high molecular weight PAHs (BaA, Ch, BbF, BkF, BaP, IP, BgP, DhA).

摘要

建立了一种高效液相色谱荧光检测法分析烤肉/鱼中 15 种多环芳烃的方法。采用甲醇/水/乙酸乙酯进行梯度洗脱。为每种 PAH 选择了最大激发和发射波长。在分析日内,保留时间的变异系数低于 0.24%,在分析日之间,变异系数低于 0.60%,非常稳定。比较了两种不同的净化和预浓缩步骤。用正己烷对 2g 冻干肉或 1g 冻干鱼进行超声辅助溶剂萃取,可获得高灵敏度、重现性和更好的萃取效率。所有 PAHs(除了 Na、Fl 和 IP,其 LOQs 低于 0.1ng/g 湿重)的定量限(LOQs,s/n=10)均低于 0.01ng/g 湿重。比较了两种不同的定量方法。标准加入法补偿了由于不完全萃取而导致的 PAHs 损失,建议用于分析通常含有极低量八种高分子量 PAHs(BaA、Ch、BbF、BkF、BaP、IP、BgP、DhA)的烤肉和烤鱼样品。

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