同位素稀释-气相色谱-质谱法测定面包中3-氯-1,2-丙二醇脂肪酸酯  

Determination of 3-chloropropane-1,2-diol esters in bread products by isotope dilution-GC-MS

作　　者：韩枫[1,2,3] 刘卿[2,3] 谢科[1,2,3] 苗虹[2,3] 吴永宁[1,2,3] 

机构地区：[1]武汉轻工大学食品科学与工程学院,武汉430023 [2]卫生部食品安全风险评估重点实验室 [3]国家食品安全风险评估中心,北京100021

出　　处：《中国科学：化学》2014年第3期389-394,共6页SCIENTIA SINICA Chimica

基　　金：国家高技术研究发展计划(2010AA023003);卫生行业公益性专项(200902009)

摘　　要：采用同位素稀释的气相色谱-质谱（GC-MS）联用技术，建立了面包中3-氯-1，2-丙二醇脂肪酸酯（3-MCPD酯）的检测方法．样品经正己烷超声提取后用甲醇钠／甲醇水解，硅藻土小柱净化，提取液经七氟丁酰咪唑（HFBI）衍生后注入GC-MS测定．目标化合物经弱极性的气相毛细管色谱柱分离，采用选择离子监测模式（SIM）监测，以同位素内标进行定量．3-MCPD酯在0．025～1．600mg／L范围内均呈良好的线性关系，相关系数（r）为0．9999，其在面包中的检出限（LOD）低至10μg／kg．以空白面包样品进行加标水平为40、100、160和240μg／kg的加标回收实验，回收率在78．9％～117．0％之间，相对标准偏差（RsD）为2．1％～4．9％，说明该方法的精密度和准确度均良好．本方法灵敏度高、定性准确，适合于面包中3-MCPD酯的检测．A method was established to detect 3-chloropropane-l,2-diol esters in bread products by gas chromatography-mass spectrometry （GC-MS）. The bakery products were ultrasonically extracted with hexane, followed by transesterification with sodium methylate/methanol, and then passed through matrix solid-supported liquid-liquid extraction （SLE） for purification. After derivatization with heptafluoro butyrylimidazole （HFBI）, 3-MCPD was determined using GC-MS. The target compounds were separated on a HP-5 capillary chromatographic column, and the tandem mass spectrograph was operated in the selected ion-monitoring mode （SIM）. There was an excellent linear correlation （r = 0.9999） between the ratio of the 3-MCPD to the internal standard and the mass in the range of 0.025-1.600 mg/L of 3-MCPD esters （calculated as 3-MCPD）. The limit of detection of 3-MCPD esters in bread products was 10 ~tg/kg. The recoveries of the 3-MCPD esters were in the range of 82.9%-113.7% at the spike levels of 40, 100, 160 and 240 ~tg/kg into blank bread products matrix, and the relative standard deviations （RSDs） were 2.1%-4.9%. The method is sensitive and accurate, which could be suitable for the determination of 3-MCPD esters in bread products.

关 键 词：同位素稀释 3-氯-1 2-丙二醇 脂肪酸酯 面包 气相色谱一质谱 

分 类 号：O657.63[理学—分析化学] TS213.21[理学—化学]