摘要:
建立了微波辅助衍生结合液相色谱-串联质谱(MAD-LC-MS/MS)同时测定水产养殖用水中硝基呋喃类代谢物3-氨基-2-唑烷基酮(AOZ)、5-甲基吗啉-3-氨基-2-唑烷基酮(AMOZ)、氨基脲(SEM)、1-氨基-2-丙酰脲(AHD)和3,5-二硝基水杨酸肼(DNSAH)的分析方法。样品经2-硝基苯甲醛微波辅助衍生1 min,乙酸乙酯提取,Acquity UPLC BEH C18色谱柱分离,以乙腈-乙酸铵(5 mmol/L,0.1%甲酸)溶液为流动相,梯度洗脱,电喷雾正负离子切换模式电离,多反应监测模式(MRM)测定。结果表明：5种代谢物在0.2~50μg/L范围内线性关系良好,相关系数均大于0.997,方法的定量限为0.02~0.05μg/L；在0.1~5μg/L的3个添加水平下,回收率在79%~102%之间,相对标准偏差(RSD)在3.6%~10.1%之间。该方法快速、简便,且易于推广,可以同时监测养殖水体中5种硝基呋喃代谢物的残留。
Abstract:
A method based on microwave-assisted derivatization (MAD)with liquid chromatography-tandem mass spectrometry (LC-MS/MS)was developed for determina-tion of 3-amino-2-oxazolidinone (AOZ ), 3-amino-5-morpholinomethy-2-oxazolidinone (AMOZ),semicarbazide (SEM),1-aminohydantoin (AHD)and 3,5-dinitrosalicylic acid hydrazide (DNSAH)in fishery water.The sample was extracted with ethyl ace-tate,then was derivatized with 2-nitrobenzaldehyde using microwave assisted method for 1 min.The analysis was carried out on an Acquity UPLC BEH C18 column by gradi-ent elution with acetonitrile-ammonium acetate (5 mmol/L,0.1% formic acid ) as mobile phase,and was detected by LC-MS/MS system with positive and negative elec-trospray ionization under multiple reaction monitoring (MRM)mode.The results show that the metabolites have good linearity in the range of 0.2-50 μg/L,and the correlation coefficients (R 2 )are better than 0.997.The limits of quantification (LOQs)of the five targets are in the range of 0.02-0.05 μg/L.The average recoveries range from 79% to 102% for the five targets at three spiked levels with the relative standard deviations of 3.6%-10.1%.The method is proved to be fast and effective for simultaneously qualita-tive and quantitative inspection of the metabolites of nitrofuran in fishery water.
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