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Determination of Heterocyclic Amines and Acrylamide in Agricultural Products with Liquid Chromatography-Tandem Mass Spectrometry

机译:液相色谱-串联质谱法测定农产品中的杂环胺和丙烯酰胺

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摘要

Heterocyclic amines (HCAs) and acrylamide are unintended hazardous substances generated by heating or processing of foods and are known as carcinogenic and mutagenic agents by the animal experiments. A simple method was established for a rapid and accurate determination of 12 types of HCAs (IQ, MeIQ, Glu-P-1, Glu-P-2, MeIQx, Trp-P-1, Trp-P-2, PhIP, AαC, MeAαC, Harman and Norharman) and acrylamide in three food matrices (non-fat liquid, non-fat solid and fat solid) by isotope dilution liquid chromatography-tandem mass spectrometry (LC-MS/MS). In every sample, a mixture of internal standards including IQ-d3, MeIQx-d3, PhIP-d3, Trp-P-2-13C2-15N and MeAαC-d3 was spiked for quantification of HCAs and 13C3-acrylamide was also spiked for the analysis of acrylamide. HCAs and acrylamide in sample were extracted with acetonitrile and water, respectively, and then two solid-phase extraction cartridges, ChemElut: HLB for HCAs and Accucat: HLB for acrylamide, were used for efficiently removing interferences such as pigment, lipid, polar, nonpolar and ionic compounds. Established method was validated in terms of recovery, accuracy, precision, limit of detection, limit of quantitation, and linearity. This method showed good precision (RSD < 20%), accuracy (71.8~119.1%) and recovery (66.0~118.9%). The detection limits were < 3.1 ng/g for all analytes. The correlation coefficients for all the HCAs and acrylamide were > 0.995, showing excellent linearity. These methods for the detection of HCAs and acrylamide by LC-MS/MS were applied to real samples and were successfully used for quantitative monitoring in the total diet study and this can be applied to risk assessment in various food matrices.
机译:杂环胺(HCA)和丙烯酰胺是通过加热或加工食品而产生的有害物质,在动物实验中被称为致癌和致突变剂。建立了一种快速,准确测定12种HCA的简单方法(IQ,MeIQ,Glu-P-1,Glu-P-2,MeIQx,Trp-P-1,Trp-P-2,PhIP,AαC同位素稀释液相色谱-串联质谱法(LC-MS / MS)测定三种食品基质(脱脂液体,脱脂固体和脂肪固体)中的MeAαC,Harman和Norharman)和丙烯酰胺。在每个样品中,均混合使用内标,包括IQ-d3,MeIQx-d3,PhIP-d3,Trp-P-2- 13 C2- 15 N和MeAαC-将d3加标以定量HCA,还加标 13 C3-丙烯酰胺以分析丙烯酰胺。样品中的HCA和丙烯酰胺分别用乙腈和水萃取,然后使用两个固相萃取柱ChemElut:用于HCA的HLB和Accucat:用于丙烯酰胺的HLB,有效去除色素,脂质,极性,非极性的干扰和离子化合物。建立的方法在回收率,准确性,精密度,检测限,定量限和线性方面得到了验证。该方法具有良好的精密度(RSD <20%),准确度(71.8〜119.1%)和回收率(66.0〜118.9%)。所有分析物的检出限均<3.1 ng / g。所有HCA和丙烯酰胺的相关系数均> 0.995,显示出极好的线性。这些通过LC-MS / MS检测HCA和丙烯酰胺的方法已应用于实际样品,并已成功地用于总膳食研究中的定量监测,并且可用于各种食品基质的风险评估。

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