高效液相色谱-柱后在线光化学衍生荧光检测法测定辣椒油中4种苏丹红染料  

Determination of four Sudan dyes in chili oil by high performance liquid chromatography with on-line photochemical derivatization and fluorescence detection

作　　者：刘珺[1] 弓振斌[1,2] 

机构地区：[1]厦门大学近海海洋环境科学国家重点实验室,福建厦门361005 [2]厦门大学海洋与环境学院,福建厦门361005

出　　处：《色谱》2012年第6期624-629,共6页Chinese Journal of Chromatography

基　　金：美国Agilent公司高等学校研究基金项目

摘　　要：建立了在线光化学衍生、荧光检测、高效液相色谱(HPLC)测定辣椒油中苏丹红Ⅰ、Ⅱ、Ⅲ和B的方法。以乙腈-水为流动相,采用梯度洗脱方式在SB-C18色谱柱上分离。用实验室自制的程序控制时间/光强光化学反应器作为在线衍生装置,优化了光衍生反应的条件和荧光检测条件。3种不同加标浓度下,辣椒油样品中4种苏丹红染料的加标回收率为81.3%～100.4%。加标水平为0.8 mg/kg下荧光信号强度的相对标准偏差(RSD,n=6)为2.6%～3.8%。苏丹红Ⅰ、Ⅱ、Ⅲ和B的检出限(LOD)和定量限(LOQ)范围分别为0.009～0.054 mg/kg和0.030～0.181 mg/kg,优于传统的HPLC分离、二极管阵列检测器检测方法。该方法具有简单、灵敏、选择性好的特点,适用于食品样品中苏丹红的常规分析。A method for the measurement of Sudan Ⅰ , SudanⅡ , Sudan Ⅲ and Sudan B in chili oil using high performance liquid chromatography （HPLC） with on-line photochemical derivatization and fluorescence detection has been developed. The Sudan dyes were separated on an SB-C18 column in a single run by the mixed mobile phase of acetonitrile-water with a gra- dient program. A laboratory-built time/energy programmed photochemical reactor （PCR） with an ultraviolet mercury lamp was installed between a photodiode array detector （PDA） and a fluorescence detector （ FLD）, and it was applied to convert the non-or weakly fluorescent Sudan dyes into fluorescence emission components. The photochemical derivatization condi- tions and fluorescence detection parameters have been investigated and optimized. The recov- eries of the standards spiked in real chili oil samples for all the dyes were 81.3% - 100.4%. The relative standard deviations （ RSDs, n = 5） of the fluorescence signal intensity at the spiked lev- el of 0.8 mg/kg were 2.6% -3.8%. The limits of detection （LODs） were in the range of 0. 009 - 0.054 mg/kg and the limits of quantification （LOQs） were 0. 030 - 0.181 mg/kg, which were better than those of the commonly used HPLC coupled with PDA. The developed method which is simple, sensitive, and selective can be applied to the routine analysis of Sudan dyes.

关 键 词：高效液相色谱法 在线光化学衍生 荧光检测 苏丹红染料 辣椒油 

分 类 号：O658[理学—分析化学]