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

Abstract

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.

Determination of Heterocyclic Amines in Meat Matrices Using Enhanced Matrix Removal‐Lipid Extraction and Liquid Chromatography–Tandem Mass Spectrometry

“…Apart from IQ, the overall recovery of HCAs conforms well to the AOAC standards, which define an acceptable recovery range as 70% to 125% for analyte concentrations at the 10 ng/g level and 75% to 120% for analyte content at 1 ng/g level in the sample (AOAC, ). The average recoveries of IQx, MeIQx, 4,8‐DiMeIQx, and PhIP using the optimized EMR‐Lipid method in our research are also comparable to values reported in the literature for the traditional Gross methods, with a recovery rate of 28.94% to 89.3% (Gibis, ; Oz & Kaya, ; Puangsombat et al., ; Smith, Ameri, & Gadgil, ), or modified methods that range from 58.2% to 107.6% (Lee et al., ; Yan et al., ), or a QuEChERS method (PSA, C18, and MgSO 4 ) ranging from 65.41& to 117.43% (Hsiao et al., ).…”

Polysaccharides Reduce Absorption and Mutagenicity of 3‐Amino‐1,4‐Dimethyl‐5H‐Pyrido[4,3‐b]Indole In Vitro and In Vivo

“…For samples from the in vivo pharmacokinetic experiment, we established an HPLC–internal standard method to analyze Trp‐P‐1. The internal standard method has been used to analyze HAAs previously (Lee and others ). In this study, PhIP was selected as the internal standard due to the similar chemical structure to that of Trp‐P‐1.…”

Review of Research into the Determination of Acrylamide in Foods

“…At the same time, the method was also applied to other food samples (bread, roasted coffee, instant coffee, cappuccino powder, and fried potatoes), and the tested AA content was lower than the EU-set level. Additionally, because of the good separation effect, LC-MS/MS can also be applied in simultaneous detection of AA and other harmful substances in one sample, which has good application value [40,41]. Wu et al used isotope-dilution ultra-performance LC-MS/MS for simultaneous detection of 4-methylimidazole and AA in 17 commercial biscuit products [42], revealing the wide presence of 4-methylimidazole and AA in biscuit products.…”