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用于高效液相色谱荧光检测法分析二甘醇的新型衍生试剂

New derivatizing reagent for analysis of diethylene glycol by HPLC with fluorescence detection.

作者信息

Wu Jiangang, Yuan Jinbin, Liu Qian, Tang Fei, Ding Li, Tan Jun, Yao Shouzhuo

机构信息

State Key Laboratory of Chemo/Biosensing & Chemometrics, Chemistry & Chemical Engineering College, Hunan University, Changsha, China.

出版信息

J Sep Sci. 2008 Dec;31(22):3857-63. doi: 10.1002/jssc.200800433.

Abstract

N-(2-Phenyl-indolyl)-acetic acid (PIAA), a new fluorescent derivatizing reagent, was used for the determination of diethylene glycol (DEG) by high-performance liquid chromatography with fluorescence detection. DEG was derivatized to ester by using PIAA in the presence of 1-ethyl-3-(3-dimethylaminopropyl)carbodimide hydrochloride (as dehydrating agent) and 4-(dimethylamino)pyridine (as base catalyst) in acetonitrile at 60 degrees C for 75 min. The influence of solvent, temperature, catalyst base, concentration of labeling reagent, and couple reagent on the derivatization was investigated. The fluorescence detection was performed with excitation at 340 nm and emission at 377 nm. Baseline separation was obtained on an Ultimate XB-C18 analytical column with water/acetonitrile gradient elution, good linearity was obtained within 0.5-50 microg/mL with a correlation coefficient of 0.9997. The limit of detection was 0.01 microg/mL (signal-to-noise ratio = 3). The method has been successfully applied to determine DEG in toothpaste samples with satisfactory recoveries ranging from 89.0 to 94.9%. The proposed method was shown to be a promising technique for the determination of DEG with high sensitivity.

摘要

N-(2-苯基吲哚基)-乙酸(PIAA)是一种新型荧光衍生试剂,用于高效液相色谱荧光检测法测定二甘醇(DEG)。在乙腈中,于60℃下,在1-乙基-3-(3-二甲基氨基丙基)碳二亚胺盐酸盐(作为脱水剂)和4-(二甲基氨基)吡啶(作为碱催化剂)存在的情况下,使用PIAA将DEG衍生化为酯,反应75分钟。考察了溶剂、温度、催化剂碱、标记试剂浓度和偶联试剂对衍生化反应的影响。荧光检测在激发波长340nm和发射波长377nm下进行。在Ultimate XB-C18分析柱上采用水/乙腈梯度洗脱实现基线分离,在0.5-50μg/mL范围内线性良好,相关系数为0.9997。检测限为0.01μg/mL(信噪比=3)。该方法已成功应用于牙膏样品中DEG的测定,回收率在89.0%至94.9%之间,结果令人满意。该方法被证明是一种测定DEG的有前途的高灵敏度技术。

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