首页> 外文期刊>Journal of chromatography, A: Including electrophoresis and other separation methods >Determination of chloramphenicol residues in meat, seafood, egg, honey, milk, plasma and urine with liquid chromatography-tandem mass spectrometry, and the validation of the method based on 2002/657/EC
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Determination of chloramphenicol residues in meat, seafood, egg, honey, milk, plasma and urine with liquid chromatography-tandem mass spectrometry, and the validation of the method based on 2002/657/EC

机译:液相色谱-串联质谱法测定肉,海鲜,蛋,蜂蜜,牛奶,血浆和尿液中的氯霉素残留量,并基于2002/657 / EC方法进行验证

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摘要

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 d(5)-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 CC alpha and CC beta were evaluated. The common CC alpha and CC beta for all matrices were 0.02 and 0.04 mu g/kg for the 321 -> 152 ion transition, and 0.02 and 0.03 Rg/kg for the 321 -> 194 ion transition. At fortification level 0.1 mu g/kg the within-laboratory reproducibility is below 25%. (c) 2006 Elsevier B.V. All rights reserved.
机译:建立了一种简单快速的LC-MS / MS法测定和确定几种食品基质中氯霉素的方法。加入d(5)-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。然后加入氯仿以除去水。蒸发后,将残留物在注入前在甲醇/水(3 + 4)中重建。在添加内标后,将尿液和血浆样品加到Chem Elut萃取柱上,用乙酸乙酯洗脱,并用己烷洗涤。蒸发后,这些样品也用甲醇/水(3 + 4)复溶。通过在负电离模式下使用MRM采集方法,将转换321-> 152、321-> 194和326-> 157分别用于定量,确认和内标。使用通用的水基校准曲线可以对氯霉素阳性样品(不考虑基质)进行定量。该方法的验证基于欧盟第2002/657号决定,并评估了计算CC alpha和CC beta的不同方法。所有基质的共同CC alpha和CC beta对于321-> 152离子跃迁为0.02和0.04μg / kg,对于321-> 194离子跃迁为0.02和0.03 Rg / kg。强化水平为0.1μg / kg时,实验室内的再现性低于25%。 (c)2006 Elsevier B.V.保留所有权利。

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