超高效液相色谱-串联质谱法测定鸡蛋中氨苄西林及其代谢物残留  

Determination of Ampicillin and Its Metabolites in Eggs by UPLC - MS / MS

作　　者：黎乃添 雍燕 叶渭源 黎健业 吴玉枝 方炳虎 LI Nai-tian;YONG Yan;YE Wei-yuan;LI Jian-ye;WU Yu-zhi;FANG Bing-hu(Guangdong Wenshi Dahuanong Biotechnology Co.,Ltd.,Yunfu,Guangdong 527400,China;South China Agricultural University,College of Veterinary Medicine,Guangzhou 510642,China;Guangdong Provincial Key Enterprise Laboratory of Veterinary Biological Products Technology Research and Application,Zhaoqing,Guangdong 526268,China)

机构地区：[1]广东温氏大华农生物科技有限公司,广东云浮527400 [2]华南农业大学兽医学院,广州510642 [3]广东省兽用生物制品技术研究与应用企业重点实验室,广东肇庆526268

出　　处：《中国兽药杂志》2024年第5期34-44,共11页Chinese Journal of Veterinary Drug

基　　金：2020年农业行业标准制修订(14202058);广东省科技计划项目(2020B1212070015);云浮市2022年科技创新项目(2022020501)。

摘　　要：建立一种同时测定鸡蛋中氨苄西林及其主要代谢物氨苄西林酸和氨苄西林二酮哌嗪的超高效液相色谱串联质谱方法。样品经乙腈水溶液(70∶30,V/V)提取、浓缩、SAX固相萃取小柱净化后,采用超高效液相色谱串联质谱法进行检测。结果显示,氨苄西林、氨苄西林酸和氨苄西林二酮哌嗪在1~200 ng/g的浓度范围内呈良好的线性关系。在鸡蛋中氨苄西林、氨苄西林酸和氨苄西林二酮哌嗪的检测限均为0.5 ng/g,定量限为1 ng/g。在1~100 ng/g添加浓度范围内,氨苄西林、氨苄西林酸和氨苄西林二酮哌嗪在鸡蛋中的平均回收率分别为84.0%~96.2%、85.6%~96.4%和89.2%~95.8%,批内、批间RSD均小于10%。添加不同浓度药物的鸡蛋样品具有良好的长期冷冻放置稳定性和反复冻融稳定性。蛋鸡在服用氨苄西林后,所产鸡蛋均能检出氨苄西林、氨苄西林酸和氨苄西林二酮哌嗪,且氨苄西林酸和氨苄西林二酮哌嗪的残留量和残留时间高于氨苄西林原型。上述内容表明,该方法各项技术指标均能满足残留检测要求,可用于定量测定鸡蛋中氨苄西林及其主要代谢物的残留量。A method of ultra high performance liquid chromatography tandem mass spectrometry was developed for the simultaneous determination of ampicillin and its main metabolites including ampicillin acid and ampicillin diketopiperazine in eggs.After extracted by acetonitrile:water(70∶30,V/V)and concentrated by rotary evaporation,the sample solution was purified by SAX solid phase extraction column,and injected into the UPLC-MS/MS system to be tested.The results showed a good linear relationship between the range of 1 to 200 ng/g concentrations for ampicillin,ampicillin acid and ampicillin diketopiperazine.The detection and quantification limit of ampicillin and its metabolites in eggs were 0.5 ng/g and 1.0 ng/g,respectively.The recoveries of ampicillin and its metabolites were 84.0%~96.2%,85.6%~96.4%and 89.2%~95.8%,and the coefficients of variation within and between the batches were less than 10%at the concentraion range of 1.0 ng/g to 100.0 ng/g.In stability experiments,the results also showed low-temperature storage stability and freeze-thaw stability of the compounds in different concentrations in eggs.The actual sample testing results show that after taking ampicillin,the eggs produced by laying hens can detect ampicillin,ampicillin acid,and ampicillin diketopiperazine,and the residual amount and residual time of ampicillin acid and ampicillin diketopiperazine are higher than those of the ampicillin.The technical indicators of this method can meet the requirements of residue testing.And the method has good reproducibility,and meets the relevant regulations of testing residues on veterinary drugs,which is suitable for for the simultaneous determination of ampicillin and its metabolites in eggs.Ampicillin,ampicillin acid,and ampicillin diketopiperazine can be detectde in the eggs produced by laying hens afeter taking ampicillin,and the residual amount and residual time of ampicillin acid and ampicillin diketopiperazine are higher than ampicillin.The technical indicators of this method can meet the requirements of re

关 键 词：鸡蛋 氨苄西林 超高效液相色谱串联质谱法 药物残留 

分 类 号：S859.84[农业科学—临床兽医学]