Study On Prepration And Application Of Enrich Material For Heterocyclic Amines In Meat Products

Heterocyclic amines (HAAs) are a kind of polycyclic aromatic compounds, formed from the protein-rich foods during hot working process. They have direct or indirect threat to people’s health for their carcinogenicity and mutagencity. Heterocyclic amines content belongs to trace levels or ultra trace level (ng g-1), so it is difficult to accurately determine their quantity.In this study, we prepared metal organic framework material as SPE sorbent and establish a HPLC method to detect five kinds of polar heterocyclic amines, including2-amino-3--methylimidazo[4,5-f]quinoline(IQ),2-amino-3,4-dimethylimidazo[4,5-f]--quinolone(MeIQ),2-amino-3,8-dimethylimidazo[4,5-f]quinoline(MeIQx),2-amino-3,4,8-dimethylimidazole-[4,5-fJ-quinoxaline (4,8-DiMeIQx),2-amino-1-methyl-6-phenyl--imidazo [4,5-b] pyridine (PhIP) using2-amino-3,4,7,8-trimethyl-imidazole[4,5-f] quinoxaline as an internal standard. The metal organic framework material MIL-101with the characters of large specific surface area, good thermal stability and a large number of unsaturated sites was synthesized by hydrothermal method and modified with amino methane sulfonic acid. The prepared materials were characterized by fourier transform infrared spectroscopy, X-ray diffraction, scanning electron microscopy and thermogravimetric analyzer. The results show.that the modified material own perfect octahedron and good thermal stability. By adsorption experiments, we can conclude that it has better adsorption and fast mass-transfer rate for selected HAAs.A new method was established using this modified material as solid-phase extraction sorbent coupling with high performance liquid chromatography (HPLC) for enrichment and detection of heterocyclic amines in meat products. Under the optimum conditions, the recoveries ranginged from72.7-108.7%, the limits of detection (S/N=3) of the method ranged from0.3-0.7μg L-1, and relative standard deviation for nine parallelled determinations were below9.67%.The linear range of IQ、MeIQ、MeIQx and4,8-DiMeIQx were0.5-100μg L-1, for PhIP was1-100μg L-1. The coefficient correlation R2ranged from0.991-0.9988, and the relative standard deviation for nine paralleled determination were below10.35%.To evaluate the application of the developed method, sauce beef, fried pork, chicken and fish loose were spiked and analyzed. The contents of IQ and4,8-DiMeIQx in fish loose were2.932and2.254μg kg-1, respectively. The contents of MeIQx in fried pork was1.537μg kg-1, the contents of PhIP in sauce beef was4.285μg kg-1. The contents of MeIQ and PhIP in chicken were3.585and5.754μg kg-1, respectively. Recoveries of the spiked sample (10,20and50μg kg-1) were achieved ranging from73.2-115.1%with satisfied relative standard deviation(RSD) of3.2-11.2%.The described method has good stability and accuracy, which can be applied in meat products to accurately detect the contents of heterocyclic amine.