气相色谱-质谱法测定酒样中多种有机锡化合物  

Determination of variety of organotin compounds in food by gas chromatography-mass spectrometry

作　　者：万益群[1,2] 马雅倩[2] 毛雪金[2] 李娟[2] 

机构地区：[1]南昌大学食品科学与技术国家重点实验室,江西南昌330047 [2]南昌大学分析测试中心,江西南昌330047

出　　处：《南昌大学学报（理科版）》2011年第4期348-352,共5页Journal of Nanchang University(Natural Science)

基　　金：国家自然科学基金资助项目(20765002;20965005);江西省科技支撑资助项目(2008BB22400);食品科学与技术国家重点实验室目标导向资助项目(SKLF-MB200807);食品科学与技术国家重点实验室自由探索资助项目(SKLF-TS-200918)

摘　　要：对白酒中的有机锡化合物运用NaBEt4进行衍生,并采用液液萃取和气相色谱-质谱法（GC-MS）对5种衍生物进行分析,建立了5种有机锡同时分析的新方法。选用选择离子扫描模式进行定性和定量分析,实验对影响反应的重要参数进行了优化。在优化条件下,5种有机锡化合物在0.01~4.0μg.mL-1的线性范围内得获得了较好的线性,检测限,相关系数为0.992 3~0.999 9,检测限为0.4~5.0μg.L-1。在0.05、0.50和4.0μg.mL-13个添加水平获得了较好的回收率,其相对标准偏差低于13.4%。该方法简便、快速、容易操作,初步运用于检测酒样中的有机锡化合物,取得较满意的结果。The organotins in spirit were derivatized with NaBEt4 and five derivatives were extracted by liquid-liquid extraction technique and analyzed by gas chromatography-mass spectrometric（GC-MS） analysis.A new method to simultaneously study the five derivatives was proposed.The qualitative and quantitative analysis of organotins was carried out by GC-MS in SIM mode.The significant factors in the experiment were optimized.The experiment parameters concerned GC separation program,sodium tetraethylborate concentration,type and volume of extraction solvent,extraction time,pH and salting out effect were optimized.Under the optimized conditions,the considerable linearties and recoveries of the organotins were obtained.The results showed the good linearity when the analytical concentration was in the range of 0.01-4.0 μg·mL-1,the linearity correlation coefficients were between 0.992 3 and 0.999 9,with the LOD in the range of 0.4-5.0 μg·L-1.The average recoveries for organotins at three different addition levels were between 68.4% and 121.0%,relative standard deviations in the range of 5.0%-13.4%、4.3%-10.6% and 4.3%-8.9% respectively.The method is proposed in this paper simple,rapid,and easy to implement for the determination of organotins in spirit.

关 键 词：有机锡 衍生化 液液萃取 气相色谱-质谱法 酒样 

分 类 号：O657.63[理学—分析化学]