微波辅助萃取-气相色谱-质谱法测定牙膏中二甘醇  

GC-MS Determination of Diethylene Glycol in Toothpaste with Microwave Assisted Extraction

作　　者：魏欢欢[1] 周剑峰[1,2] 张新春 陶冠红[1] 

机构地区：[1]苏州大学材料与化学化工学部,苏州215123 [2]江苏优联产品技术服务有限公司,苏州215128

出　　处：《理化检验（化学分册）》2010年第2期181-183,共3页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：国家自然科学基金(20345006;20575043)项目资助

摘　　要：提出了气相色谱-质谱法测定牙膏样品中二甘醇的方法。用微波萃取法以无水乙醇作萃取溶剂,在120℃萃取20min,使牙膏样品中二甘醇溶于乙醇中,所得萃取液经脱水后,用气相色谱-质谱法测定其含量。色谱分离选用HP-INNOWAX色谱柱,采用程序升温方式;质谱测定中采用电子轰击离子源及选择离子监测模式。在最佳萃取和测定条件下,方法的线性范围为0.01～50.0mg·mL-1,检出限(3s/b)为0.005mg·mL-1。用1.0mg·mL-1二甘醇标准溶液6份按方法测定,对方法的精密度作了试验,测得相对标准偏差(n=6)小于1.6%。在牙膏样品基体上加入标准溶液作回收试验,测得回收率为95.0%～103.0%。A method of GC-MS determination of diethyleneglycol in toothpaste was proposed. The sample was pre-treated by microwave assisted extraction for 20 rain at 120 ℃ using absolute alcohol as extraction solvent. After dehydration with anhydrous sodium sulfate, the extract was used for GC-MS analysis. The HP-INNOWAX capillary chromatographic column, with temperature elevation program from 130 ℃ to 250 ℃, was used in the GC separation, and the modes of electron bombardment ionization ion sourece （EI） and selective ion monitoring （SIM） were adopted in the MS measurements. Linear relationship between values of peak area and mass concentration of diethylene glycol was obtained in the range of 0. 01- 50. 0 mg · L^-1. Detection limit （3s/b） of the method was found to be 0. 005 mg · L^-1. Precision of the method was tested with 6 portions of 1.0 mg · L^-1 diethylene glycol standard solutions, value of RSD found was 1.6%. Test for recovery was made by adding standard diethylene glycol to samples of toothpaste, results found were in the range of 95.0%-103.0%.

关 键 词：气相色谱-质谱法 微波辅助萃取 二甘醇 牙膏 

分 类 号：O657.63[理学—分析化学]