固相萃取-液相色谱-串联质谱法测定莲蓉馅料中的二氧化硫脲  

Determination of thiourea dioxide in lotus seed paste fillings by solid phase extraction-liquid chromatography-tandem mass spectrometry

作　　者：汪辉[1] 曾习文 常晓途 彭新凯[1] 夏立新[1] 李亦蔚 

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 [3]长沙县食品安全检测中心,湖南长沙410100

出　　处：《色谱》2014年第1期21-25,共5页Chinese Journal of Chromatography

基　　金："十二五"国家科技支撑计划项目子课题(2012BAK17B17);湖南省科技计划重点项目(2013 WK2003)

摘　　要：建立了固相萃取-液相色谱-串联质谱法测定莲蓉馅料中违法添加的二氧化硫脲的分析方法。采用0．05％（v／v）醋酸溶液从馅料中提取二氧化硫脲，经BONDELUTPLEXA固相萃取柱（60mg／3mL）净化，采用Agilent亲水作用色谱柱（100mm×2．1mm，3．5μm）分离，以0．01mol／L醋酸铵（冰醋酸调pH至3．5）和乙腈为流动相．在多反应监测模式（MRM）下进行定性定量分析。最终，二氧化硫脲在10-1000μg／L范围内线性关系良好，检出限（LOD）和定量限（LOQ）分别为8．0μg／kg和30．0μg／kg，方法回收率为75．3％--80．7％，相对标准偏差（n：6）不超过4．83％。此方法快速、准确、特异性强、灵敏度高、样品前处理方法简便易行，适用于莲蓉馅料中二氧化硫脲的确证与测定。A method of solid phase extraction-liquid chromatography-tandem mass spectrome- try （SPE-LC-MS/MS） was developed to determine thiourea dioxide which was illegally added into lotus seed paste fillings. An amount of 0. 05% （v/v） acetic acid was used to extract thiou- rea dioxide from fillings, and the BOND ELUT PLEXA column （60 mg/3 mL） was used as the SPE column to clean-up the extraction. Then, an Agilent HILIC column （ 100 mm× 2.1 mm, 3.5 μm） was applied to separate target compounds by using the mobile phases of 0.01 mol/L ammonium acetate （ pH 3.5 ） and acetonitrile. Qualitative and quantitative analyses were opera- ted by the multiple reaction monitoring （MRM） mode. The calibration curve showed a good lin- earity for the target compound in the detection range of 10 - 1 000 μg/L. The limit of detection （LOD） and limit of quantitation （LOQ） of this method were 8.0 μg/kg and 30.0 μg/kg, respectively. The recoveries were in the ranges of 75.3% - 80.7% with the RSDs of no more than 4.83%. This proposed method was rapid, highly specific and suitable for the confirmation and quantitative determination of thiourea dioxide in lotus seed paste fillings.

关 键 词：固相萃取 液相色谱-串联质谱 二氧化硫脲 莲蓉馅料 

分 类 号：O658[理学—分析化学]