滤过型净化-超高效液相色谱-三重四极杆/复合线性离子阱质谱法测定草鱼肌肉冻干粉中4种硝基呋喃类代谢物

Determination of 4 kinds of nitrofuran metabolites in grass carp muscle lyophilized powder by pass-through cleanup-ultra performance liquid chromatography-triple quadrupole/compound linear ion trap mass spectrometry

中文关键词:  草鱼肌肉冻干粉  硝基呋喃类代谢物  滤过型净化柱  超高效液相色谱-串联质谱法

英文关键词:grass carp muscle lyophilized powder  nitrofuran metabolites  pass-through cleanup column  ultra performance liquid chromatography-tandem mass spectrometry

中文摘要:

      目的 建立一种基于滤过型净化柱净化, 结合超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)测定草鱼肌肉冻干粉中4种硝基呋喃类代谢物的快速检测方法。方法 制备阴性草鱼肌肉冻干粉作为检测目标。样品经水解、衍生化并提取浓缩后, 采用以50 mg C18为净化填料的CAFS clean-up净化柱对复溶液进行1次快速净化, 超高效液相色谱分离, 三重四极杆/复合线性离子阱质谱仪进行测定, 内标法定量分析。结果 4种硝基呋喃类代谢物在其相应的质量浓度范围内线性关系良好(r>0.999), 定量限为0.6~2.4 μg/kg; 样品中添加定量限、2.5、5.0和50.0 μg/kg浓度水平时的平均回收率在81.3%~115.1%之间, 相对标准偏差为1.5%~13.1%。结论 该方法经济、简便、高效, 灵敏度高, 重复性好, 可作为草鱼肌肉冻干粉中4种硝基呋喃类代谢物的基体标准物质的检测方法。

英文摘要:

      Objective To establish a method for the rapid determination of 4 kinds of nitrofuran metabolites in grass carp muscle lyophilized powder based on a pass-through clean-up column combined with ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods Preparation of negative grass carp muscle lyophilized powder as the detection target. After the sample was hydrolyzed, derivatized, extracted and concentrated, the complex solution was quickly purified by CAFS clean-up column with 50 mg C18 as purification filler, separated by ultra performance liquid chromatography, determined by triple quadrupole/compound linear ion trap mass spectrometer, and quantitatively analyzed by internal standard method. Results The linear relationships of the 4 kinds of nitrofuran metabolites were good within the corresponding mass concentrations (r>0.999), and limits of quantification were 0.6?2.4 μg/kg. The average recoveries of samples at spiked levels (the limit of quantification, 2.5, 5.0, 50.0 μg/kg) were 81.3%?115.1%, the relative standard deviations were 1.5%?13.1%. Conclusion This method has the advantages of economy, simplicity, high efficiency, high sensitivity and good repeatability. It can be used for the determination of matrix reference material of 4 kinds of nitrofuran metabolites in grass carp muscle lyophilized powder.