Luo W, Ang C Y, Thompson H C
Department of Health and Human Services, Food and Drug Administration, National Center for Toxicological Research, Jefferson, AR 72079-9502, USA.
J Chromatogr B Biomed Sci Appl. 1997 Jul 4;694(2):401-7. doi: 10.1016/s0378-4347(97)00171-0.
A rapid and sensitive HPLC method was developed for the determination of ampicillin residues in muscle tissues of beef, pork, chicken and catfish. Muscle tissues were blended with a food processor into paste. A 5-g aliquot of the blended tissues was homogenized with 14 ml of 0.01 M phosphate buffer (pH 4.5) using a tissue homogenizer. Proteins were precipitated with the addition of 1 ml trichloroacetic acid (75%, w/v) followed by centrifugation. After filtration, 1 ml of the supernatant was reacted with formaldehyde under acidic and heating conditions. The ampicillin fluorescent derivative was then analyzed by reverse phase HPLC with fluorescence detection. Recoveries of spiked ampicillin at 5, 10 and 20 ng/g were >85%, with coefficients of variation <5%. The limit of detection and limit of quantitation for ampicillin in the tissues were 0.6 ng/g and 1.5 ng/g, respectively. The method is also applicable to the analysis of ampicillin residue in dry milk powder.
建立了一种快速灵敏的高效液相色谱法，用于测定牛肉、猪肉、鸡肉和鲶鱼肌肉组织中的氨苄西林残留量。用食品加工机将肌肉组织搅打成糊状。取5克搅打好的组织样品，使用组织匀浆器与14毫升0.01M磷酸盐缓冲液（pH 4.5）匀浆。加入1毫升三氯乙酸（75%，w/v）使蛋白质沉淀，然后离心。过滤后，取1毫升上清液在酸性和加热条件下与甲醛反应。然后用带有荧光检测的反相高效液相色谱法分析氨苄西林荧光衍生物。添加浓度为5、10和20纳克/克的氨苄西林的回收率>85%，变异系数<5%。组织中氨苄西林的检测限和定量限分别为0.6纳克/克和1.5纳克/克。该方法也适用于分析全脂奶粉中的氨苄西林残留量。
