固相微萃取/气相色谱-质谱法测定明胶中的对羟基苯甲酸乙酯

Determination of Ethyl 4-Hydroxybenzoate in Gelatin with Solid-phase Microextraction Coupled with Gas Chromatography-Mass Spectrometry

建立固相微萃取（SPME）和气相色谱-质谱（GC—MS）联用技术测定明胶中的对羟基苯甲酸乙酯。以SPB-1701为分析柱优化了GC—MS分析对羟基苯甲酸乙酯的条件，对SPME萃取对羟基苯甲酸乙酯的条件（包括样品溶液的离子强度、萃取温度、萃取时间）以及热解析时间和温度等实验条件进行了优化。该方法测定对羟基苯甲酸乙酯的线性范围为0．05—5μg／mL，检出限为0．03μg／mL。此法可成功地用于明胶样品中对羟基苯甲酸乙酯的测定。

A technique combining solid-phase microextraction（SPME） with gas chromatography -mass spectrometry（ GC -MS） was developed to determine ethyl 4-hydroxybenzoate in gelatin. GC -MS analysis of ethyl 4-hydroxybenzoate was initially optimized by liquid injection onto an SPB-1701 column. To optimize the extraction of ethyl 4-hydroxybenzoate, several SPME parameters （ including ionic strength of sample solution, extraction time, and temperature） were examined. The desorption time and temperature were also investigated. The calibration curve of ethyl 4-hydroxybenzoate was linear in the range from 0. 05 to 5 μg/mL with a correlation coefficient of 0. 991 and the detection limit （ S/N = 3 ） was 0. 03 μg/mL. The developed SPME/GC - MS method was successfully applied to the determination of ethyl 4-hydroxybenzoate in gelatin.