固相萃取-高效液相色谱法同时测定传统禽肉制品中的9种杂环胺类化合物  

Simultaneous determination of 9 heterocyclic aromatic amines in poultry products by solid-phase extraction-high performance liquid chromatography

作　　者：邵斌[1] 彭增起[1] 杨洪生 吴光红 姚瑶[1] 万可慧[1] 

机构地区：[1]南京农业大学食品科技学院,江苏南京210095 [2]江苏省水产质量检测中心,江苏南京210017

出　　处：《色谱》2011年第8期755-761,共7页Chinese Journal of Chromatography

基　　金：国家现代农业(肉牛)产业技术体系专项项目(No.nycytx-38);江苏省科技基础设施计划项目(No.BM2008158);江苏省水产三项工程项目(No.PJ2010-52)

摘　　要：建立了固相萃取-高效液相色谱同时测定传统禽肉制品中9种杂环胺类化合物(HAAs)(包括2-氨基-3-甲基咪唑并[4,5-f]喹啉、2-氨基-3,4-二甲基咪唑并[4,5-f]喹啉、2-氨基-3,8-二甲基咪唑并[4,5-f]喹喔啉、2-氨基-3,4,8-三甲基咪唑并[4,5-f]喹喔啉、2-氨基-1-甲基-6-苯基-咪唑并[4,5-b]吡啶、3-氨基-1-甲基-5H-吡啶并[4,3-b]吲哚、3-氨基-1,4-二甲基-5H-吡啶并[4,3-b]吲哚、9H-吡啶并[4,3-b]吲哚、1-甲基-9H-吡啶并[4,3-b]吲哚)含量的分析方法。经过条件优化,肉样选用乙酸乙酯进行提取,提取液经丙基磺酸(PRS)和C18固相萃取小柱净化,采用TSK-gelODS-80TM色谱柱,以乙腈和0.05mol/L醋酸-醋酸铵缓冲液(pH3.4)为流动相进行梯度洗脱分离,紫外-荧光检测器串联方式对目标化合物进行检测。通过波长扫描,确定紫外检测波长为263nm,荧光激发波长/发射波长随时间切换程序为:0～21min,300nm/440nm;21～23.8min,315nm/410nm;23.8～35min,265nm/410nm。在上述条件下,9种HAAs在35min内实现基线分离。3个加标水平的平均回收率为60.47%～90.55%(n=6),相对标准偏差(RSD)为0.49%～9.74%(n=6),检出限(以信噪比为3计)为0.1～3.6μg/kg。该方法简便快速、结果准确、灵敏度高,可作为测定传统禽肉制品中多种杂环胺类化合物的有效方法。A method was developed for the simultaneous determination of 9 heterocyclic aromatic amines（HAAs） including 2-amino-3-methylimidazoquinoline（IQ）,2-amino-3,4-dimethylimidazoquinoline（MeIQ）,2-amino-3,8-dimethylimidazoquinoxaline（MeIQx）,2-amino-3,4,8-trimethyl-imidazoquinoxaline（4,8-DiMeIQx）,2-amino-1-methyl-6-phenylimidazopyridine（PhIP）,3-amino-1-methyl-5H-pyridoindole（Trp-p-2）,3-amino-1,4-dimethyl-5H-pyridoindole（Trp-p-1）,9H-pyridoindole（Norharman）,1-methyl-9H-pyridoindole（Harman）） in poultry products using solid-phase extraction-high performance liquid chromatography（SPE-HPLC）.The performance of 3 different organic extraction solutions,2 solid phase extraction（SPE） procedures,three different reversed-phase columns and five different mobile phases were tested for optimizing separation conditions of the 9 HAAs from poultry products.In the end,ethyl acetate was selected as the extraction solution,and the extract was purified with propylsulfonic acid silica（PRS） and C18 SPE columns.The analysis was performed on a TSK-gel ODS-80TM column using a gradient elution with the mobile phases of 0.05 mol/L aqueous acetic acid-ammonium acetate buffer（pH 3.4） and acetonitrile.The results showed that the average recoveries（n=6） of the 9 HAAs spiked in meat samples at 3 levels ranged from 60.47% to 90.55% with the relative standard deviations（RSDs） between 0.49% and 9.74%,and the limits of detection（LODs,S/N=3） were in the range of 0.1-3.6 μg/kg.The method is simple,rapid,accurate and sensitive enough for the analysis of HAAs in poultry products.

关 键 词：固相萃取 高效液相色谱 杂环胺 禽肉制品 

分 类 号：O658[理学—分析化学]