【摘要】 目的：建立顶空气相色谱-质谱联用法测定食品中亚硫酸盐含量的方法。方法：样品在顶空瓶内与磷酸介质发生反应使得产物二氧化硫（Sulfur dioxide, SO₂）溢出，在恒温下达到气液两相平衡状态。采用GS-GASPRO气相色谱柱分离，经电子轰击离子源（Electron impact ion source, EI）电离后以总离子流（Total ion current, TIC）模式进行数据采集与分析，依据保留时间及质谱信息定性，标准曲线法定量。结果：该方法在5.0～5 000.0μg/mL质量浓度范围内呈良好线性，相关系数r²=0.999,检出限（limits of detection, LODs）为0.336 mg/kg,定量限（Limits of quantitation, LOQs）为1.120 mg/kg。测得竹笋、酸菜等五种样品的加标回收率在91.3%～108.8%,相对标准偏差（Relative standard deviations, RSDs）小于6%（n=6）。应用方法对多种样品进行检测，其中蔬菜罐头类以及腌渍食品检测结果多为亚硫酸盐超标。结论：该方法前处理简单、检测时间短、精密度高，适合大批量的食品中添加剂亚硫酸盐的检测。更多还原

【Abstract】 Objective: To establish a method for the determination of sulfite in food by headspace gas chromatography-mass spectrometry（HS-GC-MS）.Methods: Sulfur dioxide（SO₂） was produced by the reaction of the sample with phosphoric acid in the headspace bottle, and reached the equilibrium state of gas-liquid phase at constant temperature.GS-GASPRO gas chromatography column was used for separation, after electron impact ion source（EI） ionization, the data were collected and analyzed by total ion current（TIC） mode.Results: The correlation coefficient of the standard working curve of this method is 0.999,the detection limit（LODs） is 0.336 mg/kg, and the quantification limit（LOQs） is 1.12 mg/kg.The recovery rates of the five samples including bamboo shoots and sauerkraut were 91.3%～108.8%,and the relative standard deviations（RSDs） was less than 6%（n=6）.The method was applied to samples, of which the test results of canned vegetables and pickled food were mostly sulfite.Conclusion: The method has the advantages of simple pretreatment, short detection time and high precision and is suitable for the determination of sulfite in large quantities of food.更多还原