食品科学 ›› 2012, Vol. 33 ›› Issue (18): 149-155.

• 分析检测 • 上一篇    下一篇

RP-HPLC-APCI MS和 RP-HPLC- ELSD法分析鸡脂甘油酯组成及结构

靳林溪,谢建春*,王 石,孙宝国   

  1. 北京工商大学 北京市食品风味化学重点实验室,食品添加剂与配料北京市高等学校工程中心
  • 收稿日期:2011-11-01 修回日期:2012-07-31 出版日期:2012-09-25 发布日期:2012-09-07
  • 通讯作者: 谢建春 E-mail:xjchun@th.btbu.edu.cn

Composition and Structural Analysis of Glycerides in Chicken Fat by HPLC-MS and HPLC-ELSD

  • Received:2011-11-01 Revised:2012-07-31 Online:2012-09-25 Published:2012-09-07

摘要: 利用反相高效液相色谱-大气压化学电离质谱(RP-HPLC-APCI MS)及反相高效液相色谱-蒸发光散射检测(RP-HPLC- ELSD)分析鸡脂甘油酯组成及结构。C18色谱柱,乙腈-二氯甲烷(60:40,V/V)为流动相,APCI MS正离子模式。根据APCI一级质谱的准分子离子及二酰基甘油碎片离子鉴定出26种甘油酯,包括4种甘油二酯和22种甘油三酯。根据二酰基甘油碎片离子的丰度高低及离子阱碰撞诱导解离产生的二级/三级碎片离子的丰度高低,判定各甘油酯中脂肪酸的位置分布。采用RP-HPLC-ELSD分析,面积归一化法定量,甘油三酯占总甘油酯的99.88%,含量最高的为1-棕榈酸-2,3-二油酸甘油酯(23.65%),其次为1-棕榈酸-2-油酸-3-亚油酸甘油酯(19.37%)、1-亚油酸-2,3-二油酸甘油酯(16.02%)。

关键词: 鸡脂, 甘油酯, 高效液相色谱, 大气压化学电离质谱, 蒸发光散射检测

Abstract: The composition and structure of glycerides in chicken fat were analyzed by reversed-phase high performance liquid chromatography-atmospheric pressure chemical ionization mass spectrometry (RP-HPLC-APCI MS) and reversed-phase high performance liquid chromatography with an evaporative light-scattering detector (RP-HPLC-ELSD). The chromatographic separation was performed on a C18 using a mobile phase of acetonitrile-methylene chloride (60:40, V/V). Glycerides were monitored by APCI MS in positive mode. According to [M+H]+ and [M+H-RCOOH]+, 26 glycerides were identified. Based on the abundance of [M+H-RCOOH]+ and ion fragments from collision induced dissociation (CID) of ion trap, the distribution of fatty acids in glycerides was deduced. Triacylglycerols represented 99.88% of total glycerides as demonstrated through RP-HPLC-ELSD analysis and quantification by peak area normalization. Among these triacylglycerols, 1-palmitoyl-2,3-di-oleoyl-glycerol revealed the highest content (23.65%), followed by 1-palmitoyl-2-oleoyl-3-linoleoyl-glycerol (19.37%), and 1-linoleoyl-2,3-di-oleoyl-glycerol (16.02%).

Key words: chicken fat, glyceride, RP-HPLC, APCI MS, ELSD