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。
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 50 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-80TMcolumn and a gradient elution with the mobile phases of acetonitrile and 0.05 mol/L acetic acidammonium 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 the10 HAAs were all above 0. 999 and thelimits of detection were in the range from 0.02 to 2.45 ng/g. The recoveries of the l0 HAAs spiked in beef samples were 61.59% - 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 jerkywere 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.
出处
《色谱》
CAS
CSCD
北大核心
2012年第3期285-291,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)
关键词
固相萃取
高效液相色谱
杂环胺
牛肉干制品
solid phase extraction （SPE）
high performance liquid chromatography （HPLC）
heterocyclic aromatic amines （HAAs）
beef jerky
