分散固相萃取-离子排斥色谱法测定食品馅料中的二氧化硫脲

Determination of thioureadioxidein and in food fillings by dispersive solid phase extractionclean-upand ion-exclusion chromatography

建立了分散固相萃取-离子排斥色谱快速测定食品馅料中二氧化硫脲的方法.样品采用0.05％乙酸溶液提取,以N-丙基乙二胺（PSA）和C18作为吸附剂的分散固相萃取法（d-SPE）进行净化,以IonPacICE-AS1（250mm×9mm,5μm）离子排阻色谱柱进行色谱分离,以50％乙腈和10mmol/L硫酸溶液为流动相,进行梯度洗脱,在紫外检测器波长269nm下检测,柱温为30℃.在0.4～ 10μg/mL范围内目标物线性关系良好（R＞0.999）,检出限（LOD,S/N≥3）和定量下限（LOQ,S/N≥10）分别为1mg/kg和3mg/kg,方法回收率在94％～ 106％之间,相对标准偏差（RSD）小于5％.该方法简单、快速、准确、重现性好,适用于食品馅料中二氧化硫脲的快速分析.

A dispersive solid phase extraction （d-SPE） clean-up andion-exclusion chromatographic method for determination of thiourea dioxide in food fillings was established. The samples were processed by 0.05% acetic acid, and purified by dispersive solid phase extraction with mixture of N-propyl ethlenediamine （PSA） and C18. The chromatographic separation was performed on an IonPac ICE-AS1 （250mm × 9mm, 5μm） column, and the column temperature was maintained at 30℃. Thiourea dioxide was detected by UV-vis detector at 269 nm. The method showed a good linearity in the range of 0.4 - 10μg/mL for Thiourea dioxide with good correlation coefficient （R 〉 0.999）. The limit of detection （LOD, S/N ≥3） was lmg/kg and the limits ofquantitation （LOQ, S/N ≥ 10） was 3mg/kg. The average recoveries of thiourea dioxide at different spiked levels were in the range of 94% - 106% with RSDs less than 5%. The result showed that the method was simple, rapid, accurate, and was suitable for the determination of thiourea dioxide in food fillings.