超高效液相色谱-串联四级杆质谱法测定水产品中硝基呋喃类代谢物的方法改进

以GB/T 20752-2006中的实验方法为基础,对超高效液相色谱-串联质谱法(UPLCMS/MS)检测水产品中呋喃它酮(AMOZ)、呋喃西林(SEM)、呋喃妥因(AHD)和呋喃唑酮(AOZ)4种硝基呋喃代谢物的样品前处理方法进行了改进。试样用0. 2 mol/L盐酸溶液溶解后,经2-硝基苯甲醛衍生化,加入0. 1 mol/L磷酸氢二钾,混匀后用1 mol/L氢氧化钠溶液调节pH约为7. 4。经乙酸乙酯直接振荡离心提取上清液,氮气吹干经超高效液相色谱串联质谱,采用正离子多反应监测(MRM)模式检测,同位素内标法定量。结果表明,四种代谢物回收率控制在90%～120%之间,RSD10%。实际样品分析结果显示,新的样品前处理方法简单、分析时间短、结果可靠,适合水产品中硝基呋喃代谢物残留的测定。

Improvement on Determination of Nitrofuran Metabolites in Aquatic ProductsUsing Ultra-high Performance Liquid Chromatography-tandem Quadrupole Mass Spectrometry

Based on GB/T 20752-2006, a sample pretreatment method for determining the four nitrofuran metabolites(Furantazone (AMOZ), Furocillin (SEM), Furantoin (AHD) and Furazolidone (AOZ)) in aquatic products by ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was optimized. The sample was dissolved in 0.2 mol/L hydrochloric acid solution, derivatized by 2-nitrobenzaldehyde, mixed with 0.1 mol/L potassium hydrogen phosphate, and adjusted the pH by 1 mol/L sodium hydroxide solution to 7.4. The supernatant was extracted by ethyl acetate direct oscillating centrifugation, dried by nitrogen, detected by ultra-high performance liquid chromatography-tandem mass spectrometry, and quantified by positive ion multi-reaction monitoring (MRM) mode and isotope internal standard method. The results showed that the recoveries of four metabolites were controlled between 90% and 120%, RSD was less than 10%. The actual sample analysis results showed that the new sample pretreatment method was simple, the analysis time was short and the results were reliable. It was suitable for the determination of Nitrofuran Metabolite Residues in aquatic products.