液相色谱-离子阱质谱联用分析食品中的对位红  

Determination of Illegal Para Red Dye in Food by HPLC-ESI MS/MS

作　　者：喻凌寒[1] 宋之光[1] 牟德海[2] 陈江韩[2] 苏流坤[2] 李光宪[2] 杨运云[2] 

机构地区：[1]中国科学院广州地球化学研究所有机地球化学国家重点实验室,广东广州510640 [2]中国广州分析测试中心广东省化学危害应急检测技术重点实验室,广东广州510070

出　　处：《分析测试学报》2006年第5期86-88,92,共4页Journal of Instrumental Analysis

摘　　要：用液相色谱／电喷雾-离子阱质谱联用建立准确测定食品中对位红染料的方法。样品中的对位红用乙腈提取，浓缩后直接进行分析。色谱柱为Agilent C18（4．0×125mm，5μm），流动相为乙腈-0．5％乙酸溶液（体积比70：30），等梯度洗脱，流速为0．5mL·min^-1，外标法定量。质谱采用正离子电离方式，选择m／z 156和277碎片离子作为定性离子，以丰度最高的碎片离子m／z 277作为定量离子。对位红染料的检出限（LOD）为1．03ng·g^-1，定量下限（LOQ）为3．08ng·g^-1；回收率为86％～112％，重复性好。本法操作简便、灵敏准确，且分析时间较短，分析周期仅需9min，适合大批样品的快速分析检测。A rapid and accurate method based on reversed-phase（RP） liquid chromatography -tandem mass spectrometry coupled with electro spray（ LC - ESI MS/MS） and an Agilent C18 4. 0 × 125 mm 5 μm column was developed to determine para red in various food samples. Samples were extracted using acetonitrile and analyzed directly upon concentration. The mobile phase was a mixture solution of acetonitrile and 0. 5% acetic acid（70 ： 30 by volume）. Mass spectrometry was operated in the positive ion mode. Ion fragments m/z 156 and m/z 277 were selected for qualitative analysis. The most abundant fragment of para red （ m/z 277 ） was chosen for quantification and to obtain a high sensitivity. The limits of detection （LOD） and quantification （LOQ） were 1.03 ng·g^-1 and 3.08 ng·g^-1, respectively, for para red in matrices. The recoveries of para red in food ranged from 86% to 112% with good reproducibility at different spiking levels. The method was applicable for rapid routine monitoring and the analytical cycle was only 9 min.

关 键 词：液质联用 对位红 食品 染料 

分 类 号：O657.63[理学—分析化学] TS202.3[理学—化学]