固相萃取-液相色谱-串联质谱法测定水产品中硝基呋喃类代谢物  

Determination of nitrofuran metabolites in aquatic products by high performance liquid chromatography tandem mass spectrometry with solid phase extraction

作　　者：陈剑刚[1] 白艳玲[1] 梁素丹 胡小玲[1] 张艳[1] 

机构地区：[1]珠海市疾病预防控制中心,广东珠海519000

出　　处：《中国食品卫生杂志》2013年第4期338-343,共6页Chinese Journal of Food Hygiene

摘　　要：目的建立水产品中呋喃它酮、呋喃西林、呋喃妥因和呋喃唑酮等硝基呋喃代谢物的固相萃取-高效液相色谱-串联质谱测定方法。方法样品中加入同位素内标,经盐酸水解及2-硝基苯甲醛衍生,再经Oasis HLB固相萃取小柱净化,乙酸乙酯洗脱吹氮浓缩;采用XTerraMS C18色谱分离柱,以乙腈-5 mmol/L乙酸铵的0.1%甲酸水溶液进行梯度洗脱,以正离子多反应监测模式,同位素内标法定量。结果 4种硝基呋喃代谢物的定量限为0.10～0.30μg/kg;方法的线性范围为0.5～25μg/kg,r>0.995;代谢衍生物的加标回收率分别为81.0%～104.8%、91.0%～110.3%、85.0%～111.4%和88.0%～108.2%;RSD在2.7%～14.5%之间。应用建立的方法对180份淡水鱼进行测定,其中4份检出3-氨基-2-噁唑烷基酮(AOZ),含量为1.3～3.6μg/kg。结论方法选择性高、灵敏,能满足水产品中硝基呋喃类代谢物残留的高灵敏分析。Objective The method for determination of metabolites of four nitrofuran antibiotics,nitrofurantoin（AMOZ）,furaltadone（SEM）,nitrofurazone（AHD） and furazolidone（AOZ） in aquatic products was developed by solid-phase extraction coupled with liquid chromatography tandem mass spectrometry（LC-MS/MS）.Methods Samples with isotope internal standard solutions were hydrolyzed by HCl and derivatized with 2-nitrobenzaldehyde.The analytes were cleaned up on HLB solid-phase column and eluted with ethyl acetate,then evaporated and dried with nitrogen gas.The extract components were separated and gradient eluted on a XTerra C18 column with acetonitrile-5 mmol/L ammonium acetate of 0.1% formic acid solutions ion,and simultaneously quantified by the isotope internal standard operating in positive ion under multiple reactions monitoring mode.Results The limits of quantification ranged from 0.10 μg/kg to 0.30 μg/kg for four nitrofuran metabolites.The standard curves were linear in the range of 0.5-25 μg/kg,with the correlation coefficients0.995.The average recoveries for nitrofuran metabolites were 81.0%-104.8%,91.0%-110.3%,85.0%-111.4%,88.0%-108.2% respectively,and their relative standard deviation varied between 2.7% and 14.5%.The method was applied to analyze 180 fish samples from Guangdong region,four of which were confirmed to contain AOZ ranging from 1.3 to 3.6 μg/kg.Conclusion The method developed was selective,sensitive and accurate,completely suitable for nitrofuran metabolites trace analysis in aquatic products.

关 键 词：液相色谱-串联质谱 硝基呋喃类代谢物 固相萃取 水产品 兽药残留 

分 类 号：R155.5[医药卫生—营养与食品卫生学]