共轭亚油酸检测方法
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Cognis GmbH , Standort Illertissen
AMIA-000010 安全-健康-环境-质量
分析方法E- IA -000010 (第二版第二版))
用气相色谱法定量测定用气相色谱法定量测定下列的游离的脂肪酸下列的游离的脂肪酸
C16:0,棕榈酸 C18:0,硬脂酸 C18:1 c9,油酸 C18:2 c9, c12,亚油酸 C18:2, 共轭亚油酸(总和) C18:2, c9,t11,共轭亚油酸异构体 C18:2, t10,c12,共轭亚油酸异构体 C18:2, c,c ,共轭亚油酸异构体 C18:2, t,t ,共轭亚油酸异构体 脂肪酸乙酯 CLA-低聚物
含有游离脂肪酸的混合物
IA-001010 前版本:1071 IA-002010 前版本:1171 IA-003010 前版本:1271 IA-004010 前版本:1371 IA-005010 前版本:1471 IA-006010 前版本:1571 IA-007010 前版本:1671 IA-008010 前版本:1771 IA-009010 前版本:1871 IA-010010 前版本:1971 IA-011010 前版本:2071
(硅烷化后使用非极性的色谱柱)
替代分析方法替代分析方法::E-IA-1071-2071,第一版本
有效期起始日有效期起始日:: 2004年07月23日
归档归档::2009年07月
内容目录内容目录::
1. 用途和/或应用范围·······················································································2
2. 定义·················································································································2
3. 概述·················································································································2
4. 试剂·················································································································2
5. 仪器·················································································································2
6. 取样·················································································································2
7. 程序·················································································································2
8. 评估·················································································································3
9. 文献·················································································································4 批准人:
1. 用途和/或应用领域
本方法用于定量检测脂肪酸混合物的组成,特别是定量检测共轭亚油酸(CLA )的组成及其副产物。这个方法没有关于测定C18:2 c11,t13脂肪酸的含量的信息。
2. 定义
“Oligomers ”-即低聚物,可以理解为在脂肪酸共轭反应过程当中的高分子量的产物(其组成还没有确定)。
3. 概要概要
样品在干燥嘧啶中,在添加了MSTFA 的作用下发生硅烷化反应,硅烷化反应的产物通过气相色谱的毛细管柱进行分离,使用FID 检测器并且进行定量。定量结果使用面积百分比(A%)进行表示。
4. 试剂试剂
(1)干燥嘧啶(pyridine),水分含量不超过0.01%
(2)MSTFA(N-Methyl-N-T-rimethyllilyl-trifluoraceramide)
5. 仪器和材料仪器和材料
5.1 5.1 样品制备需要的仪器样品制备需要的仪器样品制备需要的仪器
(1)1.5ml 的GC 自动进样瓶。 (2)加热块
5.2 5.2 气相色谱气相色谱GC GC,,
(1)气相色谱仪,GC-系统6850 (2)自动进样器6850
(3)色谱柱: 毛细管DB 5HT,15m, 0.32mm I.D., 0.1um 膜厚度 (4)检测器: FID
(5)进样器: 分流进样器
6. 取样取样
按照标准操作规程进行取样。
7. 操作程序操作程序 7.1.
安全安全::
应注意处理危险物品的具体细则。技术、组织和个人安全测定方法应遵守。
7.2. 样品制备样品制备::
(1)称取14mg 的样品(精确到0.01mg)加入到GC 自动进样器的安瓿瓶中(单个测试)。
(2)加入1ml 的嘧啶和100ul 的MSTFA。 (3)放在80℃的加热块上加热10min。