摘要
采用溶胶 凝胶方法制备了25,27 二羟基 26,28 (1′,10′ 二氧代 4′,7′ 二氮杂 3′,8′ 二氧代亚辛基) 对 特丁基 杯[4]芳烃/羟基硅油(胺桥杯[4]/OH TSO)固相微萃取(SPME)探头,通过对脂肪胺和芳胺的分析研究了它的特性。该探头具有耐高温、抗溶剂冲洗、使用寿命长、重现性好等特点。杯环上极性胺桥的引入增强了涂层的极性,因而在不需衍生的情况下对脂肪胺和芳胺都具有很好的萃取能力,表现出对胺类化合物的特殊选择性。脂肪胺的检出限为0 19～39 51μg/L,线性范围达3个数量级,相对标准偏差(RSD)≤5 1%;芳胺的检出限为1 21～40 73ng/L,线性范围达4～6个数量级,RSD≤6 0%。将此SPME技术与气相色谱联用能简单、快速、有效地检测鱼的鲜度。
A novel solid-phase microextraction (SPME) fiber coated with 25,27-dihydroxy-26, 28-(1′,10′-dioxa-4′,7′-diaza-3′,8′-dioxooctylene)-p-tert-butylcalix[4]arene/hydroxy-terminated silicone oil (amide bridged -C[4]/OH-TSO) was prepared with sol-gel technology and applied to the analysis of aliphatic amines and aromatic amines without derivatization. It demonstrated high thermal stability of up to 380 ℃ and stability in organic and inorganic solvents, a prolonged lifetime of over 200 times for headspace SPME, great fiber-to-fiber reproducibility with a relative standard deviation (RSD) of no more than 6.3% for aromatic amines, etc. Due to the introduction of polar amide bridge in calixarene molecules, polarity of the coating increases and thus the fiber shows better extraction efficiency in most of the investigated aliphatic amines and aromatic amines compared to the extraction efficiency of commercial fibers, indicating specific selectivity and sensitivity to amines. The detection limits (LODs) were determined to be 0.19-39.51 μg/L, the linear ranges were 3 orders of magnitude with a precision better than 5.1% for aliphatic amines, and they were 1.21-40.73 ng/L, 4-6 orders of magnitude with a precision better than 6.0% for aromatic amines. The application of this SPME technique coupled with gas chromatography has been shown to be feasible for the rapid determination of fish freshness.
出处
《色谱》
CAS
CSCD
北大核心
2004年第5期472-475,共4页
Chinese Journal of Chromatography
基金
国家自然科学基金资助项目(No.20375028).
关键词
气相色谱
固相微萃取
杯芳烃
脂肪胺
芳胺
鱼
gas chromatography
solid-phase microextraction
calixarene
aliphatic amines
aromatic amines
fish
