固相萃取-高效液相色谱法同时测定羊肉制品中9种杂环胺  

Simultaneous determination of nine heterocyclic aromatic amines in mutton products by solid phase extractionhigh performance liquid chromatography

作　　者：郭海涛[1] 潘晗[1] 王振宇[1] 陈丽[1] 张德权[1] 

机构地区：[1]中国农业科学院农产品加工研究所,农业部农产品加工综合性重点实验室,北京100193

出　　处：《色谱》2012年第10期1074-1080,共7页Chinese Journal of Chromatography

基　　金：公益性行业(农业)科研专项课题(200903043-01-06);国家科技支撑计划项目(2012BAD29B03-05)

摘　　要：建立了同时测定羊肉制品中9种杂环胺的固相萃取-高效液相色谱(SPE-HPLC)分析方法。样品经2 mol/LNaOH超声提取、80 mL二氯甲烷液-液萃取,利用阳离子交换柱(MCX柱)净化和富集后进行HPLC分析。采用反相C18色谱柱,以乙腈和0.01 mol/L磷酸溶液(用三乙胺调整pH 3.6)为流动相对杂环胺进行梯度洗脱,使用二极管阵列检测器(DAD)分别在228 nm(2-氨基-9H-吡啶并[2,3-b]吲哚(AaC)、2-氨基-3-甲基-9H-吡啶并[2,3-b]吲哚(MeAaC))、253 nm(2-氨基-3-甲基咪唑并[4,5-f]喹啉(IQ)、1-甲基-9H-吡啶并[3,4-b]吲哚(Harman)、2-9H-吡啶并[3,4-b]吲哚(Norharman))、263 nm(2-氨基-3,8-二甲基咪唑并[4,5-f]喹喔啉(MeIQx)、2-氨基-3,4,8-三甲基咪唑并[4,5-f]喹喔啉(4,8-DiMeIQx)、3-氨基-1-甲基-5H-吡啶并[4,3-b]吲哚(Trp-p-2))、321 nm(2-氨基-1-甲基-6-苯基咪唑并[4,5-b]吡啶(PhIP))处进行检测。实验结果表明,9种杂环胺分离效果良好,回收率为50.27%～94.77%(n=6),相对标准偏差为0.08%～4.42%;通过全波长扫描,确定检出限(以信噪比(S/N)=3计)为1.6～41.0μg/L。该方法操作简单,结果准确,重现性好,可用于同时检测羊肉制品中9种杂环胺的含量。A method was established for the simultaneous determination of nine heterocyclic aromatic amines（HAAs） in mutton products by solid phase extraction-high performance liquid chromatography（SPE-HPLC）.As a result,the sample was prepared by ultrasound in 2 mol/L NaOH,and dichloromethane was selected as the extraction solvent.The extract was purified and concentrated with an MCX SPE column.The chromatographic separation was achieved on a reverse-phase C18 column by gradient elution using 0.01 mol/L phosphoric acid（adjusted to pH 3.6 by triethylamine） and acetonitrile,detected with a diode array detector（DAD） at 228 nm for 2-amino-9H-pyridoindole（AaC） and 2-amino-3-methyl-9H-pyridoindole（MeAaC）;253 nm for 2-amino-3-methylimidazoquinoline（IQ）,1-methyl-9H-pyridoindole（Harman）,9H-pyridoindole（Norharman）;263 nm for 2-amino-3,8-dimethylimidazoquinoxaline（MeIQx）,2-amino-3,4,8-trimethylimidazoquinoxaline（4,8-DiMeIQx）,3-amino-1-methyl-5H-pyridoindole（Trp-p-2）;321 nm for 2-amino-1-methyl-6-phenylimidazopyridine（PhIP）.The results showed that the nine HAAs can be separated efficiently.The recoveries（n=6） of the nine HAAs spiked in meat were between 50.27% and 94.77% with the relative standard deviations of 0.08%-4.42%.The limits of detection of this method were 1.6-41.0 μg/L for the nine HAAs.The method is simple,accurate,rapid and repeatable.It can be used for the simultaneous determination of the nine HAAs in mutton products.

关 键 词：固相萃取 高效液相色谱 杂环胺 羊肉制品 

分 类 号：O658[理学—分析化学]