离子对液相色谱法测定食品馅料中的二氧化硫脲

Determination of thiourea dioxide in food stuffing by ion-pair liquid chromatography

建立了高效液相色谱法测定食品馅料中二氧化硫脲的检测方法。样品中的二氧化硫脲经稀盐酸超声提取后，以AthenaC18-wp柱（250mm×4．6mm，5um）为分析柱，甲醇和0．0025mol／L四丁基硫酸氢铵溶液为流动相，采用二级管阵列检测器，在269nm波长下进行检测，紫外光谱定性，外标法定量。二氧化硫脲在0．004×0．120g／L质量浓度范围内与其峰面积呈良好线性关系，线性相关因子R=0．9999。以3倍信噪比所相当的含量值为检出限，方法最低检出限为5×10-4／kg。4种空白样品在2个不同加标水平下的回收率均在103％～112％之间，相对标准偏差RSD均小于4％。该方法可用于食品馅料中二氧化硫脲的检测分析。

A method based on high performance liquid chromatographic （HPLC） has been developed for detecting thiourea dioxide （TD） in food stuffing. The samples were extracted with hydrochloric acid solution by ultrasonic. The separation and quantifica- tion of TD were conducted on an Athena C18-wp column （250 mm × 4. 6 mm, 5 land at 269 nm with mobile phase of methyl and 0. 002 5 mol/L tetrabutyl ammonium hydrogen sulfate. Lab-buih UV spectroscopy library and external standard were employed for the identification and quantification of target compounds. The results indicated that the calibration curves of TD showed a good linear relationship between peak areas and mass concentrations in the range of 0. 004 0. 120 g/L with correlation coefficients more than 0. 999 9. The limit of detection （LODs, S/N 3） was 5× 10 -4 g/kg. The recoveries of four blank stuffing samples at three spiked concentration levels ranged from 103%-112% with relative standard deviations （RSDs） below 4%. Therefore, this method can be used for detecting and quantifying thiourea dioxide in food stuffing.