液液萃取-高效液相色谱-电感耦合等离子体质谱联用检测黄酒中的有机锡  

Determination of Multi-Organotion Compounds in Yellow Rice Wine by Liquid-Liquid Extraction-High Performance Liquid ChromatographyIductively Coupled with Plasma Mass Spectrometry

作　　者：范洋波[1] 吴坚[1] 郑云峰[1] 李博斌[1] 葛乐勇[1] 金晶[1] 

机构地区：[1]绍兴市质量技术监督检测院,国家黄酒产品质量监督检验中心,浙江绍兴312071

出　　处：《酿酒科技》2014年第11期90-93,共4页Liquor-Making Science & Technology

基　　金：浙江省分析测试科技计划项目(2011C37070)

摘　　要：利用高效液相色谱-电感耦合等离子体质谱联用技术（HPLC-ICP/MS）对黄酒中4种重要的有机锡[三甲基锡（TMT）、三苯基锡（TPT）、二丁基锡（DBT）、三丁基锡（TBT）]进行了分离和检测。采用Agilent TC-C18柱进行有机锡的形态分析，流动相为V（乙腈）：V（水）：V（乙酸）=（70：20：10，φ），0.05%的三乙胺，pH 3.5，流速为0.6 mL/min，测定了1～200μg/L范围内4种有机锡化合物的混合标准工作曲线，其相关系数优于0.998（R2），方法的检测限都在0.1μg/L左右。用乙腈（NaCl）、二氯甲烷、甲苯分别萃取黄酒中的有机锡后，用上述方法进行分析。结果表明，被测黄酒中有三甲基锡（TMT）被检出，含量为17.5μg/L ，用乙腈萃取黄酒中的有机锡，萃取效果最佳，4种有机锡的加标回收率均达到80%以上。The hyphenated technique of high performance liquid chromatography coupled plasma mass spectrometry（HPLC-ICP-MS）was applied for the determination of four organotion compounds [trimethyltin （TMT）,triphenyltin （TPT）,dibutyltin （DBT）,tributyltin （TBT）] in yellow rice wine. Agilent TC-C18 column was used for the separation,the mobile phase of HPLC was V（CH3CN）：V（H2O）：V（CH3COOH）=（70：20：10,φ）, 0.05%TEA ,and pH was adjusted to 3.5. The flow rate was 0.6 mL/min.Four mix standard solution from 1 to 200 μg/L were applied for the method assessment.The experimental results indicated that, the correlation coefficient of calibration curves（R2） for each organotin compound was over 0.998 and the detection limits of the four organotin compounds were about 0.1μg/L.The Organotion Compounds were extracted by acetoni-trile（CH3CN）,carbon dichloride （CH2Cl2） and methylbenzene（C7H8） from yellow rice wine respectively.And the extracted-liquid were determinated by HPLC-ICP/MS.The results showed that TMT was determinated in yellow rice wine and its content was17.5 μg/L. The extracted organotin compounds from rice wine by acetonitrile（CH3CN） had the best recoveries of over 80%.

关 键 词：高效液相色谱-电感耦合等离子体质谱法 有机锡 黄酒 萃取 

分 类 号：O657.63[理学—分析化学] TS262.4[理学—化学]