基于PRiMEHLB前处理技术的鸡蛋中四环素类药物的.docx

基于PRiME HLB前处理技术的鸡蛋中四环素类药物的
快速筛选方法研究
张婧基金项目:上海市科委科研计划项目(**********)
作者简介:张婧,女,助理畜牧师,硕士,研究方向为动物性产品中药物残留检测研究。
通讯作者:李丹妮。E-mail: jingzhang0209@
,潘娟,严凤,吴剑平,李丹妮*
上海市兽药饲料检测所,上海 201103;
摘要:本实验使用新型固相萃取小柱PRiME HLB处理鸡蛋样品,建立了一种鸡蛋中四种四环素类药物的简单、快速的筛选分析方法。鸡蛋样品经Na2EDTA-Mcllvaine 缓冲液提取,乙***沉淀蛋白,PRiME HLB固相萃取柱净化,浓缩富集后,采用液相色谱法检测,外标法定量。PRiME HLB固相萃取法是简单的通过式净化处理方法,样品净化过程简单、快速、高效。方法最低检出限为50 μg/kg,定量限为100 μg/kg,土霉素、四环素、金霉素、多西环素4种四环素类药物在50~5000 ng/mL范围内呈现良好线性,回收率满足分析筛选的要求。该方法可以有效起到快速筛选鸡蛋中四环素类药物残留的作用,具有较广的应用性。
关键词:PRiME HLB;四环素类药物;液相色谱;鸡蛋
PRiME HLB based effective screening method for Tetracyclines in eggs
ZHANG Jing1, PAN Juan, YAN Feng, Wu Jian-ping, Li Dan-ni*
Shanghai Municipal Institute of Veterinary Drug and Feedstuff Control,Shanghai 201103,China
Abstract: An effective screening method for Tetracyclines in eggs was developed. This highly performance liquid chromatography (HPLC) method was based on the new solid phase extraction column, PRiME HLB. The pounds in eggs were extracted with Na2EDTA-Mcllvaine buffer solution, defatted with acetonitrile, then through PRiME HLB, and finally quantified by external standard method after concentration. The PRiME HLB could be applied without activation for purifying the
tetracyclines in eggs, which brought out the pretreatment simple, fast, and effective. The method showed a good linear relationship in the range of 50 to 5000 ng/mL, with a LOD of 50 μg/kg, and a LOQ of 100 μg/kg, and the recovery met the requirement for screening. These results presented that the study would be effective and would open a new application of screening tetracyclines in eggs.
Key words: PRiME HLB; Tetracyclines; ultra performance liquid chromatography; egg
四环素类抗生素(Tetracyclines,TCs) 是一种广谱抗菌素,因其抗菌性好、价格低廉,这类药物常被用于畜禽疾病的预防和治疗。兽医临床上常用的主要有四环素(TC)、金霉素(CTC)、土霉素(OTC)、多西环素(DOTC)等[1-2]。目前我国仅批准金霉素和土霉素可以作为饲料添加剂使用,而四环素和多西环素不允许作为饲料添加剂使用[3]。但是一些养殖户为了追求经济效益,长期违规或超标使用此类抗生素,造成药物残留[4-5]。这不仅会影响兽药的治病疗效,也会给食用者的身体健康带来严重危害[6-7]。
我国针对四环素、金霉素、土霉素三种四环素类药物规定了在禽蛋中的最大残留限量为200 μg/kg[