色谱

色谱 ›› 2012, Vol. 30 ›› Issue (03): 285-291.DOI: 10.3724/SP.J.1123.2011.11039

• 研究论文 • 上一篇    下一篇

高效液相法测定牛肉干制品中10种杂环胺含量

万可慧, 彭增起*, 邵斌, 姚瑶, 石金明   

  1. 南京农业大学食品科技学院, 江苏 南京 210095
  • 收稿日期:2011-11-21 修回日期:2011-12-28 出版日期:2012-03-28 发布日期:2012-05-02
  • 通讯作者: 彭增起,博士,教授,博士生导师,主要从事肉品加工与质量控制研究.
  • 基金资助:

    国家现代农业(肉牛)产业技术体系专项项目(No.nycytx-38).

Determination of 10 heterocyclic aromatic amines in beef jerky by high performance liquid chromatography

WAN Kehui, PENG Zengqi*, SHAO Bin, YAO Yao, SHI Jinming   

  1. College of Food Science and Technology, Nanjing Agricultural University, Nanjing 210095, China
  • Received:2011-11-21 Revised:2011-12-28 Online:2012-03-28 Published:2012-05-02

PDF

439

摘要：

建立了固相萃取-高效液相色谱同时分析牛肉干制品中10种杂环胺含量的方法。样品经二氯甲烷(含5%甲苯)萃取,丙基磺酸(PRS)柱和C18固相萃取小柱净化后,以甲醇-氨水定容,经TSK-gel ODS-80TM色谱柱分析,采用乙腈和0.05 mol/L醋酸-醋酸铵缓冲液(pH 3.5)作为流动相进行梯度洗脱,紫外-荧光检测器的串联方式检测杂环胺含量。结果表明,10种杂环胺在线性范围内线性关系良好,相关系数r＞0.999,检出限为0.02～2.46 ng/g。杂环胺的加标回收率为61.69%～101.81%,相对标准偏差(RSD)为0.28%～7.81%。8种市售牛肉干制品中均检测出1-甲基-9H-吡啶并［4,3-b］吲哚(Harman)和9H-吡啶并［4,3-b］吲哚(Norharman),可测杂环胺总量为16.65～60.38 ng/g。该方法线性范围广,灵敏度高,净化效果好,可满足实际样品分析的需求。

关键词: 高效液相色谱, 固相萃取, 牛肉干制品, 杂环胺

Abstract:

An analytical method was developed for the simultaneous determination of 10 heterocyclic aromatic amines (HAAs) in beef jerky by solid phase extraction-high performance liquid chromatography (SPE-HPLC). The HAAs were eluted from an Extrelut NT 20 SPE column with 60 mL dichlormethane (containing 5% toluene), and then the extract was purified with a propylsulfonic acid silica (PRS) column and a C18 SPE column, and finally, the HAAs were stored in a methanol-ammonia solution. The separation was achieved by using a TSK-gel ODS-80TM column and a gradient elution with the mobile phases of acetonitrile and 0.05 mol/L acetic acid-ammonium acetate buffer (pH 3.5). The identification and quantitative analysis of the HAAs fraction were carried out using an HPLC system with ultraviolet-fluorescence detectors. The results showed that the correlation coefficients of the 10 HAAs were all above 0.999 and the limits of detection were in the range from 0.02 to 2.46 ng/g. The recoveries of the 10 HAAs spiked in beef samples were 61.69%~101.81% with the relative standard deviations (RSDs) between 0.28% and 7.81%. 1-Methyl-9H-pyrido［4,3-b］indole (Harman) and 9H-pyrido［4,3-b］indole (Norharman) were detected in all beef jerky, and the total HAAs content of beef jerky were between 16.65 and 60.38 ng/g. This method is with wide linear range and high sensitivity, and is enough for the analysis of the HAAs in actual meat samples.

Key words: beef jerky, heterocyclic aromatic amines (HAAs), high performance liquid chromatography (HPLC), solid phase extraction (SPE)