Rønning Helene Thorsen, Einarsen Kristin, Asp Tone Normann
Norwegian School of Veterinary Science, Section for Food Safety, P.O. Box 8146-Dep. 0033 Oslo, Norway.
J Chromatogr A. 2006 Jun 23;1118(2):226-33. doi: 10.1016/j.chroma.2006.03.099. Epub 2006 Apr 24.
A simple and rapid method for the determination and confirmation of chloramphenicol in several food matrices with LC-MS/MS was developed. Following addition of d5-chloramphenicol as internal standard, meat, seafood, egg, honey and milk samples were extracted with acetonitrile. Chloroform was then added to remove water. After evaporation, the residues were reconstituted in methanol/water (3+4) before injection. The urine and plasma samples were after addition of internal standard applied to a Chem Elut extraction cartridge, eluted with ethyl acetate, and hexane washed. Also these samples were reconstituted in methanol/water (3+4) after evaporation. By using an MRM acquisition method in negative ionization mode, the transitions 321-->152, 321-->194 and 326-->157 were used for quantification, confirmation and internal standard, respectively. Quantification of chloramphenicol positive samples regardless of matrix could be achieved with a common water based calibration curve. The validation of the method was based on EU-decision 2002/657 and different ways of calculating CCalpha and CCbeta were evaluated. The common CCalpha and CCbeta for all matrices were 0.02 and 0.04 microg/kg for the 321-->152 ion transition, and 0.02 and 0.03 microg/kg for the 321-->194 ion transition. At fortification level 0.1 microg/kg the within-laboratory reproducibility is below 25%.
建立了一种用液相色谱-串联质谱法测定和确证多种食品基质中氯霉素的简单快速方法。加入氘代氯霉素作为内标后,用乙腈提取肉、海鲜、鸡蛋、蜂蜜和牛奶样品。然后加入氯仿去除水分。蒸发后,残渣用甲醇/水(3+4)复溶后进样。尿液和血浆样品加入内标后应用于Chem Elut萃取柱,用乙酸乙酯洗脱,并用己烷洗涤。这些样品蒸发后也用甲醇/水(3+4)复溶。在负离子模式下采用多反应监测采集方法,分别用321→152、321→194和326→157的离子对进行定量、确证和内标。无论基质如何,氯霉素阳性样品的定量都可以用普通的水基校准曲线实现。该方法的验证基于欧盟第2002/657号决定,并评估了计算CCalpha和CCbeta的不同方法。对于321→152离子对,所有基质的通用CCalpha和CCbeta分别为0.02和0.04微克/千克,对于321→194离子对,分别为0.02和0.03微克/千克。在0.1微克/千克的加标水平下,实验室内的重现性低于25%。