色谱2012,Vol.30Issue(3):285-291,7.DOI:10.3724/SP.J.1123.2011.11039
高效液相色谱法测定牛肉干制品中10种杂环胺
Determination of 10 heterocyclic aromatic amines in beef jerky by high performance liquid chromatography
摘要
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 prop-ylsulfonic 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-80? 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%. L-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.关键词
固相萃取/高效液相色谱/杂环胺/牛肉干制品Key words
solid phase extraction (SPE)/ high performance liquid chromatography (HPLC)/ heterocyclic aromatic amines (HAAs)/ beef jerky分类
化学化工引用本文复制引用
万可慧,彭增起,邵斌,姚瑶,石金明..高效液相色谱法测定牛肉干制品中10种杂环胺[J].色谱,2012,30(3):285-291,7.基金项目
国家现代农业(肉牛)产业技术体系专项项目(No.nycytx-38). (肉牛)