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投稿时间:2024-03-15
投稿时间:2024-03-15
中文摘要: 硝基呋喃代谢物现有的检测方法前处理过程复杂、试验流程长,无法达到批量高效检测的要求。该文采用单一变量法逐步优化前处理过程,简化试验流程,建立动物源食品中硝基呋喃代谢物的液相色谱-串联质谱高效检测的方法。样品经盐酸酸化、高温衍生、氢氧化钠调节pH值、低温高速离心、乙酸乙酯萃取、氮吹复溶、滤膜过滤,采用液相色谱-串联质谱检测。对猪肉和鱼肉进行0.5、1.0、3.0 μg/kg 3个水平的加标回收试验,回收率在81.1%~107.4%,精密度小于9.7%。对禽畜肉、水产品、鸡蛋等进行1.0 μg/kg加标回收试验,回收率在83.5%~114.0%,精密度小于9.5%。该优化后的检测方法操作简单、准确度高、稳定性好、通用性高,适用于多基质动物源食品中硝基呋喃代谢物的高效检测,可推广应用于农产品的批量检测中。
Abstract:The existing methods for detecting nitrofuran metabolites mostly involve complex pretreatment processes and lengthy experimental procedures,which fail to meet the requirements for efficient batch detection.In this study,the single-variable method was used to gradually optimize the pretreatment process. The experimental process was simplified. An efficient detection method for nitrofuran metabolites in animal-derived foods was established by liquid chromatography-tandem mass spectrometry. The samples were acidified with hydrochloric acid and derivatized at high temperatures. The sample's pH was adjusted with sodium hydroxide,and then the sample was centrifuged at low temperatures and high speeds. The liquid supernatant was extracted with ethyl acetate,re-dissolved after nitrogen blowing,and filtered through a filter membrane. The extracted residues were analyzed with liquid chromatography-tandem mass spectrometry. The spiked recovery experiments were conducted on pork and fish at three levels of 0.5,1.0,and 3.0 μg/kg. The average recoveries were between 81.1% and 107.4%. The precision was less than 9.7%. The spiked recovery experiments were also performed on poultry and livestock meat,aquatic products,and eggs at 1.0 μg/kg. The recoveries were between 83.5% and 114.0%. The precision was less than 9.5%. The optimized detection method was simple to operate,highly stable,and versatile. The method was suitable for the efficient detection of nitrofuran metabolites in animal-derived foods with multiple matrices and could be widely applied to batch testing of agricultural products.
keywords: animal-derived food nitrofuran metabolite liquid chromatography-tandem mass spectrometry optimization efficient detection
DOI:10.12161/j.issn.1005-6521.2025.18.019
文章编号:202518019 中图分类号: 文献标志码:
基金项目:
| Author Name | Affiliation |
| WANG Qianqian | Yantai Testing Center for Food and Drug,Yantai 264000,Shandong,China |
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