A selective biomarker for confirming nitrofurazone residues in crab and shrimp using ultra-performance liquid chromatography–tandem mass spectrometry
A selective biomarker for confirming nitrofurazone residues in crab and shrimp using ultra-performance liquid chromatography–tandem mass spectrometry
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使用超高效液相色谱-串联质谱法确认螃蟹和虾中呋喃西林残留的选择性生物标志物
DOI：
10.1007/s00216-015-9058-7
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发表时间：
2015-10
影响因子：
4.3
通讯作者：
Xiaojun Zhang
中科院分区：
文献类型：
--
作者：
Shuai Zhang;Yuanming Guo;Zhongyong Yan;Xiumei Sun;Xiaojun Zhang
养殖蟹和虾中呋喃西林残留的可靠检测以前受到缺乏适当的具体分析方法的阻碍。母体NFZ在肉类中迅速分解，而常用的侧链代谢物氨基脲（SEM）是非特异性的，因为它天然存在于甲壳动物壳中，经常导致肉类中的“假阳性”检测。以5-硝基-2-糠醛（NF）为标记代谢物，经2，4-二硝基苯肼（DNPH）柱前衍生化，超高效液相色谱-串联质谱（LC-MS/MS）负离子电喷雾电离模式下的超高效液相色谱-串联质谱（UPLC-MS/MS）分析能够确认有意处理的全蟹、蟹肉和虾肉中的NFZ残留，检测限（LOD）和定量限（LOQ）低于1 ng g−1。同时，首次合成了DNPH-NF衍生物，并通过制备液相色谱法进行了纯化，用核磁共振谱（1H-NMR）对其结构进行了表征。用超高效液相色谱-紫外可调（UPLC-TUV）法检测衍生物的纯度，含量均在99.9%以上。为了比较的目的，甲壳类动物样品进行了分析，使用NF和SEM标记代谢物。NF和SEM标记代谢物都显示了NFZ处理，但未处理的螃蟹也显示出可测量的SEM水平，这可能被误解为非法使用NFZ的证据。
Reliably detecting nitrofurazone (NFZ) residues in farmed crab and shrimp was previously hindered by lack of appropriately specific analytical methodology. Parent NFZ rapidly breaks down in meat, and the commonly used side-chain metabolite, semicarbazide (SEM), is non-specific as it occurs naturally in crustacean shell often leading to ‘false positive’ detections in meat. Using 5-nitro-2-furaldehyde (NF) as marker metabolite, following pre-column derivatization with 2,4-dinitrophenylhydrazine (DNPH), ultra-performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) analysis in negative electrospray ionization mode enabled confirmation of NFZ residues in deliberately treated whole crab, crab meat and shrimp meat, with a limit of detection (LOD) and limit of quantification (LOQ) below 1 ng g−1. Meanwhile, the derivatives of DNPH-NF were synthesized for the first time, purified by preparative liquid chromatography and structure characterized with nuclear magnetic resonance spectroscopy (1H-NMR). The purity of derivative was checked by ultra-performance liquid chromatography–tunable ultraviolet (UPLC–TUV), and the contents were beyond 99.9 %. For comparison purposes, crustacean samples were analysed using both NF and SEM marker metabolites. NFZ treatment was revealed by both NF and SEM marker metabolites, but untreated crab also showed measurable levels of SEM which could potentially be misinterpreted as evidence of illegal NFZ use.Graphical abstractConfirmation of nitrofurazone residues in crab
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影响因子：
3.3
作者：
S. Szilágyi;M. B. de la Calle
通讯作者：
S. Szilágyi;M. B. de la Calle
影响因子：
6.1
作者：
Chu, Pak-Sin;Lopez, Mayda I.;Plakas, Steven M.
通讯作者：
Plakas, Steven M.
DOI：
10.1080/02652030701586657
发表时间：
2008-05-01
期刊：
FOOD ADDITIVES AND CONTAMINANTS
影响因子：
--
作者：
Cooper, K. M.;Mccrack-En, R. J.;Kennedy, D. G.
通讯作者：
Kennedy, D. G.
影响因子：
6.1
作者：
C. Van Poucke;Christ'l M. Detavernier;M. Wille;J. Kwakman;P. Sorgeloos;C. V. Van Peteghem
通讯作者：
C. Van Poucke;Christ'l M. Detavernier;M. Wille;J. Kwakman;P. Sorgeloos;C. V. Van Peteghem
影响因子：
8.8
作者：
R. McCracken;Bob Hanna;D. Ennis;L. Cantley;Dermot Faulkner;D. Glenn Kennedy
通讯作者：
R. McCracken;Bob Hanna;D. Ennis;L. Cantley;Dermot Faulkner;D. Glenn Kennedy