亲水作用色谱法快速筛查食品馅料中违法添加的二氧化硫脲  

Rapid Screening of Thiourea Dioxide in Food Fillings by Hydrophilic Interaction Liquid Chromatography

作　　者：汪辉[1] 彭新凯[1,2] 夏立新[1] 章建辉 李莎 周探春 

机构地区：[1]长沙市食品质量安全监督检测中心,湖南长沙410013 [2]湖南省食品安全生产工程技术研究中心,湖南长沙410013

出　　处：《分析测试学报》2014年第7期804-809,共6页Journal of Instrumental Analysis

基　　金："十二五"国家科技支撑计划项目子课题(2012BAK17B17);湖南省科研条件创新专项计划(2012TT1008)

摘　　要：建立了亲水作用色谱快速筛查食品馅料中违法添加的二氧化硫脲的分析方法。采用0．05％醋酸溶液冰水浴超声提取二氧化硫脲，离心后经0．45μm微孔滤膜过滤后上机测试。采用亲水型色谱柱Venusil HILIC（4．6mm×250mm，5μm）分离，柱温为25℃，以0．02mol／L醋酸铵（冰醋酸调至pH4．5）和乙腈为流动相，梯度洗脱，经二极管阵列检测器分析，检测波长为275nm。二氧化硫脲在6．0～200mg／L范围内线性关系良好，检出限（LOD）和定量下限（LOQ）分别为22．5mg／kg和75．0mg／kg，方法回收率为92．7％～107％，相对标准偏差（RSD，n=6）为0．53％～3．8％。方法快速、准确、重现性好，适用于食品馅料中二氧化硫脲的快速筛查。A hydrophilic interaction liquid chromatographic method was established for rapid screen- ing of thiourea dioxide illegally added in food fillings. 0. 05% acetic acid was used for ultrasonic extraction of thiourea dioxide in ice water bath. The extraction solution was centrifuged natant was tested after filtered through 0. 45μm cellulose micro pore membrane. , and the super- The target corn- pound was separated on a Venusil HILIC （4. 6 mm × 250 mm, 5μm） column at 25 ℃, using 0. 02 mol/L ammonium acetate （glacial acetic acid adjust pH 4.5 ） - acetonitrile as mobile phase by gradi- ent elution, and detected with photodiode array detector at 275 nm. The calibration curve showed a good linearity for thiourea dioxide within the range of 6.0 -200 mg/L. The limits of detection （LOD） and limits of quantitation（LOQ） for the method were 22. 5 mg/kg and 75.0 mg/kg, respectively. The spiked recoveries of thiourea dioxide in food fillings ranged from 92.7% 0. 53% -3.8%. This method was rapid, accurate and repeatable, and screening thiourea dioxide in food fillings to 107% with RSDs of was suitable for rapid

关 键 词：亲水作用 高效液相色谱(HPLC) 食品馅料 二氧化硫脲 

分 类 号：O657.7[理学—分析化学] F407.82[理学—化学]