超高效液相色谱-串联质谱法检测罗非鱼中喹乙醇及其衍生物

Determination of olaquindox and its derivatives in tilapia mossambica by ultra high pressure liquid chromatography-mass spectrometry

中文关键词:  喹乙醇  3-甲基-喹噁啉-2-羟酸  罗非鱼  超高效液相色谱-串联质谱法

英文关键词:olaquindox  methyl-3-quinoxaline-2-carboxylic acid  tilapia mossambica  ultra performance liquid chromatography-tandem mass spectrometry

中文摘要:

      目的 建立超高液相色谱-串联质谱法(ultra high pressure liquid chromatography-mass spectrometry, UPLC-MS/MS)测定罗非鱼中喹乙醇(olaquindox, OLQ)及其代谢物3-甲基-喹噁啉-2-羧酸(3-methyl-quinoxaline-2-carboxylic acid, MQCA)含量的分析方法。方法 样品经10 mL 50%甲醇溶液50 ℃水浴超声提取, PPL固相萃取小柱净化, 经2 mL去离子水淋洗、2 mL 60%甲醇溶液洗脱, 以乙腈-0.1%甲酸为流动相, 经syncronis C18色谱柱分离, 采用多反应监测正离子模式进行定性及定量分析。结果 OLQ和MQCA在0.01～5.0 μg/mL范围内线性关系良好, 相关系数(r2)均大于0.998, 检出限为0.003 mg/kg和0.001 mg/kg, 定量限为0.01 mg/kg和0.003 mg/kg, OLQ的3个水平加标回收率为87.0%～98.0%, RSD为3.3%～4.7%; MQCA的3个水平加标回收率为79.0%～84.0%, RSD为1.4%～3.6%。结论 该方法具有灵敏度高、重复性好、准确度高、样品前处理操作简便和检测速度快的优点, 适用于罗非鱼中喹乙醇及其代谢物MQCA快速高效定量、定性分析。

英文摘要:

      Objective To establish a method for determination of olaquindox?and?its metabolite?3-methyl- quinnoxaline-2-carboxylic acid (MQCA) in tilapia mossambica by ultra pressure liquid chromatography-mass spectrometry. Methods The samples were extracted by 10 mL 50% methanol solution in 50 ℃ water bath, purified by PPL solid phase extraction column, eluted by 2 mL deionized water and 2 mL 60% methanol solution, separated by syncronis C18 column with acetonitrile-0.1% formic acid as mobile phase, and analyzed qualitatively and quantitatively by multi-reaction monitoring positive ion mode. Results The linear relationship between OLQ and MQcA was good in the range of 0.015.0 μg/mL, the correlation coefficient (r2) was greater than 0.998, the detection limit was 0.003 mg/kg and 0.001 mg/kg, the quantitative limit was 0.01 mg/kg and 0.003 mg/kg, the recovery rate of three levels of OLQ was 87.0%98.0%, the RSD was 3.3%4.7%, and the recovery rate of three levels of MQCA was 79.0%84.0%, the RSD was 1.4%3.6%. Conclusion This method has the advantages of high sensitivity, good repeatability, high accuracy, easy operation of sample pretreatment and fast detection speed. It is suitable for rapid and efficient quantitative and qualitative analysis of olaquindox and its metabolite MQCA in tilapia mossambica.