快速蒸馏-高效液相色谱荧光法测定食品中二氧化硫  

Determination of Sulfur Dioxide in Food by Rapid Distillation and High Performance Liquid Chromatography Fluorescence Method

作　　者：温艳梅 曾义福 方沛 卢桃 周洁 王仕平 WEN Yanmei;ZENG Yifu;FANG Pei;LU Tao;ZHOU Jie;WANG Shiping(Jiangxi Yichun Inspection and Testing Center,Yichun,Jiangxi 336000,China)

机构地区：[1]江西省宜春市检验检测中心,江西宜春336000

出　　处：《农产品加工》2025年第5期68-71,共4页Farm Products Processing

基　　金：宜春市科技计划项目(JXYC2021KSB027)。

摘　　要：为建立快速蒸馏-高效液相色谱荧光法检测食品中的二氧化硫。样品经蒸馏仪快速蒸馏酸化产生二氧化硫,被氢氧化钠溶液吸收生成亚硫酸盐,亚硫酸盐与衍生试剂邻苯二甲醛(OPA)-铵盐在pH值6.8条件下反应,生成强荧光物质1-磺酸基-异吲哚。色谱条件:流动相为甲醇-水(70∶30,V∶V),柱温40℃,流速1.0 mL/min,激发波长320 nm,发射波长380 nm,荧光检测器检测,外标法定量。结果表明,在质量浓度0.1016~4.0640μg/m L内具有良好线性关系,相关系数R^(2)为0.9999,检出限为2.2μg/L,相对标准偏差(RSD)为1.67%~3.91%,加标回收率为91.57%~101.15%。该方法快速准确,适用于测定食品中的二氧化硫残留量。To establish a method for determination of sulfur dioxide in food by rapid distillation and high performance liquid chromatography fluorescence method.The sample was rapidly distilled and acidified by a distillation apparatus to produce sulfur dioxide,and the volatilized SO2 was absorbed by the sodium hydroxide solution.The absorbed sulfite,ammonium salt and ortho-phthalaldehyde(OPA)could react to generate isoindole-1-sulfonate with strong fluorescence in a medium with a pH of 7.0,detected with fluorescence detector with the mobile phase of methanol-water(70∶30,V∶V)with column temperature 40℃,and the flow rate was 1.0 mL/min.The excitation wavelength was set at 320 nm and the emission wavelength was set at 380 nm.The external standard method was used for quantification.The results showed that good linearity was showed when the concentration of sulfur dioxide was among 0.1016~4.0640μg/mL with the linear correlation coefficient R^(2) was 0.9999,and the detection limit was 2.2μg/L;The relative standard derivation(RSD)was among 1.67%~3.91%,and the average adding standard recovery rate was between 91.57%~101.15%,with the precision and accuracy meeting the detection requirement.The method was rapid and accurate,which was suitable for detection of sulfur dioxide residues in food.

关 键 词：快速蒸馏 高效液相色谱荧光法 食品 二氧化硫 

分 类 号：R155.5[医药卫生—营养与食品卫生学]