摘要
利用高效液相色谱-串联质谱（HPLC-MS/MS）联合改进的QuEChERS建立了同时测定活海参中硝基呋喃类药物的代谢物氨基脲、1-氨基乙内酰脲、3-氨基-2-唑烷基酮、5-甲基吗啉-3-氨基-2-唑烷基酮的方法。样品经盐酸水解，2-硝基苯甲醛衍生，37 ℃水浴16 h，调节至pH 7.0 ~7.5，QuEChERS提取净化，氮吹至干后，用20%乙腈水定容，经C18色谱柱分离，以乙腈-0.1%甲酸溶液为流动相进行梯度洗脱，用HPLC-MS/MS以多反应监测模式进行检测。结果表明，该方法的线性范围为1.0 ~10 μg/L，4种代谢物的相关系数均不小于 0.999，检出限和定量下限分别为0.15 μg/kg 和0.5 μg/kg，在0.5，1.0，2.0，5.0 μg/kg的加标水平下，回收率为88.0%~109.6%，相对标准偏差（RSD）为3.8% ~11.0%。用此方法对大连地区200批海参进行检测，合格率为95%。该方法前处理操作简便，省时，溶剂消耗量小，可作为同时分析活海参中4种硝基呋喃类药物代谢物残留量的有效手段。
A high performance liquid chromatography-tandem mass spectrometry（HPLC-MS/MS）combined with QuEChERS method was developed for the simultaneous qualitative and quantitative analyses of four metabolites of nitrofuran antibiotics,including semicarbazide（SEM）,1-amino-hydantoin（AHD）,3-amino-2-oxazolidinone（AOZ）,5-morpholino-3-amino-2-oxazolidone（AMOZ）.The samples were hydrolyzed with HCl,and derivatized with 2-nitrobenzaldehyde at 37 ℃ for 16 h.The derivative solutions were adjusted to pH 7.0-7.5.The analytes were extracted and pured by Bond Elut QuEChERS.The separation was carried out on a C18 column,using acetonitrile-0.1% formic acid as mobile phase by gradient elution.The analytes were detected by tandem mass spectrometry with electrospray ionization source under multiple reaction monitoring（MRM） mode.The method showed a good linearity between peak area ratios of the analytes to the internal standard and concentration of the analytes with correlation coefficients all above 0.999 over the dynamic range of 1.0-10 μg/L.The limits of detection（LODs） and quantitation （LOQs） of four antibiotics were 0.15 μg/kg and 0.5 μg/kg,respectively.The average recoveries of all the compounds at four spiked levels of 0.5,1.0,2.0,5.0 μg/kg ranged from 88.0% to 109.6% with RSDs （n=6） of 3.8%-11.0%.This method was used to detect 200 batches of holothurian in Dalian with the passing percentage of 95%.Compared to the traditional pretreatment method,this method is more easy to operate and less solvent comsuming,and is proved to be fast and effective for the simultaneous qualitative and quantitative analyses of the metabolites of nitrofuran antibiotics in holothurian.
出处
《分析测试学报》
CAS
CSCD
北大核心
2016年第9期1127-1131,共5页
Journal of Instrumental Analysis
关键词
硝基呋喃代谢物
QUECHERS
海参
高效液相色谱-串联质谱
nitrofuran metabolites
QuEChERS
holothurian
high performance liquid chromatography tandem mass spectrometry（HPLC-MS/MS）
