牛肉中阿莫西林残留的高效液相色谱分析11.docVIP

牛肉中阿莫西林残留的高效液相色谱分析 摘要：建立了反高效液相色谱分析牛肉样品中阿莫西林残留量的方法。对动物组织样品采用磷酸盐缓冲溶液提取、三氯乙酸沉淀蛋白、固相萃取净化和富集。研究了样品在C18柱上的保留行为和阿莫西林的特征谱图。待测物用高效液相色谱法分离，外标定法定量分析，标准曲线的线性良好,相关系数为0.99934，线性范围为5.0～500ug/L。动物组织样品中阿莫西林的加标回收率为77.3％～97.4％，相对标准偏差为1.2％～13.5％，最低检出限低于10ug/kg。该分析方法具有良好的重现性。 关键词：高效液相色谱；固萃取；阿莫西林；残留量；牛肉 Determination of Amoxicillin Residue in Beeves by High Performance Liquid Chromatography Abstract: A reversed-phase high performance liquid chromatographic method﹙RP-HPLC﹚ has been developed for the determination of amoxicillin residue in beeves. Beeves were extracted using phosphate buffer, precipitated proteins with trichloroacetic acid ﹙TCA﹚ solution, cleaned up with and enriched by solid phase extraction ﹙SPE﹚.The retention behaviors on a C18 column and the Chromatography condition of amoxicillin were investigated. The samples were separated by RP-HPLC and quantified using external standard calibration curves.There were good linear correlations ﹙the correlation coefficient was 0.99934﹚between the peak areas and concentrations of amoxicillin .The dynamic linear range was 5.0-500μg/mL.The average recoveries of amoxicillin in spiked animal tissues ranged from 77.3％ to 97.4％, and the relative standard deviations were between 1.2％ and 13.5％. The limit of detection was below 10ug/kg. The relative standard deviations of intra-assay and inter-assay were both within 10％. This analysis method has good recurrence. Key word：HPLC;solid phase extraction;amoxicillin; residue;Beeves 阿莫西林﹙amoxicillin﹚,化学名称为羟氨苄青霉素，属于青霉素类β-内酰胺抗生素，医学和兽医临床应用广泛。抗生素的应用给畜牧业生产的发展做出了巨大的贡献，饲用抗生素可抑制畜禽消化道内有害微生物的生长和繁殖，增强畜禽的抗病能力，防止疾病，减少体内营养消耗，节省维生素和蛋白质等，使肠壁变薄，从而有利于营养成分的渗透与吸收，增进食欲，同时可刺激脑下垂体分泌激素，促进发育。但是抗生素引起的内源性感染、二重感染、细菌耐药性的产生、畜禽免疫力的下降和畜产品药物残留等问题都对饲料工业、养殖业和人类健康带来了负面影响。而阿莫西林的过量使用会导致人体内白血球降低，影响内脏功能，发生脏器损害等，对老年人、儿童，特别是胎儿的影响更大，严重者会导致胎儿病变、畸形、流产、死亡。由于过敏反应和细菌产生耐药性等原因，目前阿莫西林残留是欧盟、北美等国家可食性动物产品进出口中的必检项目之一，而且要求非常严格：欧盟要求在动物的肌肉、肝、肾、脂肪中的阿莫西林的最高限量为0.05mg/kg;美国要求更低，为0.01mg/kg。 目前，对于该药的分析测定方法主要包括高效液相色谱法、酸碱滴定法、紫外分光光度法、导数广谱法、流动注射-原子吸收光谱法、免疫分析法和微生物测定