基于气相色谱法定量分析二氧化硫

Quantitative Analysis of Sulfur Dioxide Based on Gas Chromatography

本文研发了一种测定食品中二氧化硫(SO_(2))的气相色谱-质谱法。首先,将样品放入200 g/L NaCl溶液中超声提取,然后离心,取上清液并加入顶空瓶中(含H_(2)SO_(4)溶液)。食品中的SO2在80℃的酸性条件下反应并生成,同时在气相和液相中实现平衡。利用气相色谱柱GS-GASPRO对气相部分进行分离,然后利用离子扫描(SIM)模式采集数据,以进行定量和定性分析。大批量食品中的SO_(2)均可采用此方法进行定量和定性测定,相关系数在2.5~100μg范围内为0.9999,6类典型食品经过加标实验后(3种不同浓度),当添加量为25.0~250 mg/kg时,RSD与回收率分别为0.38%~6.4%、90.1%~104.4%,此方法的检出限为3.0 mg/kg。

This article developed a gas chromatography-mass spectrometry method for the determination of sulfur dioxide(SO_(2))in food.Firstly,place the sample in a 200 g/L NaCl solution for ultrasonic extraction,then centrifuge,take the supernatant and add it to a headspace bottle(containing H_(2)SO_(4)solution).SO_(2)in food reacts and generates under acidic conditions at 80℃,achieving equilibrium in both gas and liquid phases.Separate the gas phase using gas chromatography column GS-GASPRO,and then collect data using ion scanning(SIM)mode for quantitative and qualitative analysis.This method can be used for quantitative and qualitative determination of SO_(2) in large quantities of food.The correlation coefficient ranges from 2.5μg to 100μg is 0.9999.The RSD and recovery rate of 6 typical foods were 0.38%to 6.4%and 90.1%to 104.4%,respectively,when added at a mass of 25.0~250 mg/kg after spiking experiments(3 different concentrations).The detection limit of this method is 3.0 mg/kg.