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.
出处
《分析测试学报》
CAS
CSCD
北大核心
2006年第5期86-88,92,共4页
Journal of Instrumental Analysis
