National Reference Laboratory of Veterinary Drug Residues (HZAU), Huazhong Agricultural University, Wuhan 430070, PR China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2010 Dec 15;878(32):3415-20. doi: 10.1016/j.jchromb.2010.10.028. Epub 2010 Oct 30.
A specific and sensitive method based on liquid chromatography-tandem mass spectrometry (LC-MS/MS) has been developed for the determination of nitrovin and sodium nifurstyrenate residues in muscle and liver of swine and chicken and in muscle of fish. Sample preparation procedure includes ultrasound-assisted extraction with acetonitrile, defatting with n-hexane and final clean-up with solid phase extraction (SPE) on Oasis HLB cartridges. The analytes were detected in multiple reaction monitoring (MRM) under negative scan mode acquiring two diagnostic product ions for sodium nifurstyrenate and under positive mode for nitrovin. The averaged decision limits (CCα; α 1%) ranged 0.09-0.26 μg/kg while the detection capability (CCβ; β 5%) was 0.33-0.97 μg/kg in the tissues. Reasonable recoveries (71-110%) spiked in muscle and liver showed excellent relative standard deviation (RSD). The validated method was simple, rapid, sensitive, and complied with the regulations for the determination of nitrovin and sodium nifurstyrenate residues in food matrices.
一种基于液相色谱-串联质谱（LC-MS/MS）的特异性和灵敏性方法已被开发出来，用于检测猪、鸡肌肉和肝脏以及鱼类肌肉中的硝呋烯钠和硝基呋喃代谢物残留。样品制备程序包括用乙腈进行超声辅助提取、用正己烷脱脂，最后用 Oasis HLB 固相萃取小柱进行净化。分析物在负扫描模式下的多重反应监测（MRM）中检测，硝呋烯钠采用两个诊断产物离子，硝基呋喃采用正模式检测。组织中平均决策限（CCα；α=1%）为 0.09-0.26μg/kg，检测能力（CCβ；β=5%）为 0.33-0.97μg/kg。肌肉和肝脏中添加的回收率合理（71-110%），相对标准偏差（RSD）良好。验证后的方法简单、快速、灵敏，符合食品基质中硝基呋喃和硝呋烯钠残留量的测定规定。
