| Heterocyclic amines,mainly occur in the protein food through heat treatment,especially in meat products,and also can be found in the environment,human body fluids,water and so on,so it is unavoidable for people to be exposed to various types of heterocyclic amines every day.Heterocyclic amines have a strong carcinogenic mutagenicity,long-term contact damage to the human body.However,it usually exists in products at the very low level such as μg L-1.Besides,the food matrix is complex,which contains a lot of protein,fat and other impurities,these issues have greatly limited the study and analysis of heterocyclic amines.Therefore,the analysis and detection of heterocyclic amines have been concerned by many scholars.Firstly,the liquid chromatography tandem mass spectrometry method was used to detect the content of heterocyclic amines in 24 kinds of barbecue and meat sauce products from three different regions（Beijing,Tianjin,Shijiazhuang）.2-amino-3-methylimidazo[4,5-f]quinoline（IQ）,2-amino-3,4-dimethylimidazo[4,5-f]quinoline（MeIQ）,2-amino-3,8-dimethyli-midazo[4,5-f]quinoxaline（MeIQx）,2-amino-3,4,8-trimethylimidazo[4,5-f]quinoxaline（4,8-DiMeIQx）and 2-amino-l-methyl-6-phenylimidazo[4,5-b]pyridine（PhIP）that are common and harmful to human health were detected.The results showed that the samples from Beijing area have the highest level in the total heterocyclic amines,and samples from Shijiazhuang area have more types of heterocyclic amines than from other areas.Secondly,the analysis method for heterocyclic amines was established using the molecularly imprinted polymers which have selective adsorption property for heterocyclic amines as solid phase adsorbent,and coupled with high performance liquid chromatography-UV detector.According to the structure of the selected object heterocyclic amines,3-Amino-9-ethylcarbazole（AEC）was selected as dummy template,methacrylic acid（MAA）as a functional monomer,ethylene glycol dimethacrylate hydroxyethyl methacrylate（EGDMA）as a functional monomer,and azobisisobutyronitrile（AIBN）as the initiator to synthesize a highly selective imprinted polymer material on the surface of the silicon sphere modified with double bond.The resultant materials were obtained under the optimum synthesis conditions,and were also characterized by Fourier infrared spectroscopy,electron microscopy,adsorption equilibrium experiment,and adsorption kinetics experiment.The synthesized surface imprinted polymer was used as an adsorbent for solid phase extraction,and the optimum conditions were obtained by optimizing the sample solvent,elution solvent and elution volume.Under the optimal conditions,the linear range of five kinds of heterocyclic amines is 1-100 μg L-1 the correlation coefficient is above 0.99.The detection limit of the method was in the range of 0.31-0.55 μg L-1.The method is applied to the actual sample,select roast duck,pork liver,and stewed drumstick purchase fromTianjin local supermarket,in the roast duck can be detected MeIQ and MeIQx and concentrations were 2.739 μg kg-1 and 1.581 μg kg-1,detected MeIQx as 3.472μg kg-1 in the pork liver;in stewed drumstick can be detected concentration as 2.265 μg kg-1 PhIP.Three kinds of practical samples were low,medium,high(20,40,60 μg kg-1)three levels.The recovery rate of five kinds of heterocyclic amines was 67.13%-111.37%,RSD<9.42%.The method is expected to be used for the detection of real samples. |
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