郑晓菊， 许泳吉*， 刘云云， 韩玮
（青岛科技大学 化学与分子工程学院，山东 青岛 266042）
摘要： 利用柱前衍生高效液相色谱法测定了贝壳类海洋生物（蛤蜊、牡蛎、扇贝）中多胺（主要是指亚精胺（SPD）和精胺（SPM））的含量。采取多种提取试剂(如不同浓度的HCl和H2SO4、甲醇、水提醇沉等)考察了样品中多胺的提取效果，另外，确定了最佳提取时间和温度。结果表明：样品中多胺的最佳提取条件为6 mol·L-1HCl溶液，蛤蜊和牡蛎60 ℃下提取3 h，扇贝提取时间4 h为好。提取液用丹磺酰氯衍生，甲苯萃取后高效液相色谱分析。色谱条件：流动相为甲醇和水，采用梯度洗脱，柱温40 ℃，荧光检测。测定结果：亚精胺（SPD）的回归方程为Y=0172 9+0261 6 X（R=0998 8），检出限为048 pmol；精胺（SPM）的回归方程Y=0074 0+0170 4X（R=0999 2），检出限为054 pmol。
关键词： 高效液相色谱； 贝类； 多胺； 提取方法
中图分类号： Q 966 文献标志码： A
Determination of Polyamine in Shelled Marine Creatures by High Performance Liquid Chromatography (HPLC)
ZHENG Xiaoju， XU Yongji， LIU Yunyun， HAN Wei
（College of Chemistry and Molecular Engineering， Qingdao University of Science and Technology， Qingdao 266042， China）
Abstract: This experiment used precolumn derivatization HPLC to determine Polyamine content in shelled marine creatures (clams, oysters, scallops). The polyamine mainly refered to is spermidine (SPD) and spermine (SPM).We took a variety of extraction reagent, such as different concentrations of HCl and H2SO4, methanol, water alcohol sink, etc, and inspected the extraction effect of polyamine in the sample. In addition, extraction time and temperature were determined. The experimental result showed that the optimum extraction conditions of polyamines in samples was 6 mol·L-1HCl solution at 60 ℃ for 3 h, which only scallops extraction time is 4 h for good. This extract used HPLC to analysis with dansyl chloride derivatization after toluene extraction. The chromatographic conditions: the mobile phase of methanol and water, using gradient elution, the column temperature was 40 ℃, fluorescence detection. The determination results:the regression equation of the spermine (SPD):Y=0172 9+0261 6X（R=0998 8）， the detection limit is 048 pmol; The regression equation of the spermine (SPM)： Y=0074 0+0170 4X（R=0999 2）， the detection limit is 054 pmol.
Key words: HPLC; shelled marine creatures; polyamine; extraction method
收稿日期： 20130718
作者简介： 郑晓菊(1988—)，女，硕士研究生. *通信联系人.
