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作 者:王丹[1] 谷翠梅 李琳[1] 葛辉[1] WANG Dan;GU Cui-mei;LI Lin;GE Hui(Clinical Laboratory,Weifang Center for Disease Control and Prevention,Weifang,Shandong 261061,China)
机构地区:[1]潍坊市疾病预防控制中心检验科,山东潍坊261061
出 处:《中国卫生工程学》2023年第1期17-19,23,共4页Chinese Journal of Public Health Engineering
基 金:山东省潍坊市卫健委科研项目(WFWSJK-2022-141)。
摘 要:目的建立EMR-Lipid QuEChERS超高效液相色谱/串联质谱法测定动物源性食品中氯霉素及4种硝基呋喃代谢物残留量的检测方法。方法采用EMR-Lipid前处理方法、UPLC-MS/MS分析技术,测定动物源性食品中氯霉素及4种硝基呋喃代谢物残留量。结果不同空白基质样品中分别添加0.5、1.0、5.0、10.0μg/kg的氯霉素、4种硝基呋喃代谢产物的混合标准溶液,不同基质的加标回收率皆在52.6%~85.2%范围,相对标准偏差(RSD)在3.6%~17.2%范围。动物组织空白基质中线性回归方程的相关系数r分别为0.905~0.999、表明经过EMR-Lipid QuEChERs方法处理过的氯霉素、4种硝基呋喃代谢产物在0.5~50.0μg/L范围内线性关系良好。以3倍信噪比计算得到检出限为0.02~0.05μg/kg,10倍信噪比算得定量限为0.06~1.50μg/kg。结论用EMR-Lipid QuEChERs快速方法净化,能将目标物有效提取,过程简单,节约试剂和时间成本,各项指标也均满足相关法规的要求,可以作为研究动物源性食品中氯霉素及4种硝基呋喃代谢产物残留量的检测方法。Objective This paper aims to establish a method for the determination of chloramphenicol and four nitrofuran metabolites in food of animal origin by QuEChERS UPLC-MS/MS.Methods QuEChERS pretreatment method and UPLC-MS/MS analysis technology were used.Results After 0.5,1.0,5.0 and 10.0μg/kg were added to different blank matrix samples of mixed standard solution of chloramphenicol and four nitrofuran metabolites,the recoveries of different substrates were in the range of 52.6%-85.2%,with relative standard deviation(RSD)in the range of 3.6%-17.2%.The correlation coefficient r of the linear regression equation in the blank matrix of animal tissue was 0.905-0.999 respectively,indicating that the linear relationship of chloramphenicol and four nitrofuran metabolites treated by EMR lipid QuEChERS was good in the range of 0.5-50.0μg/L.The detection limit calculated by 3 times signal-to-noise ratio was 0.02-0.05μg/kg,while the quantitative limit by 10 times signal-to-noise ratio was 0.06-1.50μg/kg.Conclusion The rapid method of EMR lipid QuEChERS can effectively extract the target,with simple process,saving reagent and time cost.All indexes also meet the requirements of relevant laws and regulations.It can be used as a method to study the residues of chloramphenicol and four nitrofuran metabolites in animal derived foods.
关 键 词:QUECHERS 超高效液相色谱/串联质谱法 动物源性食品 氯霉素 硝基呋喃代谢物残留
分 类 号:Q657.7[生物学—生物物理学] R155.5[医药卫生—营养与食品卫生学]
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