高效液相色谱-串联质谱法测定猪肝中硝基呋喃类代谢物残留

    Determination of nitrofuran metabolite residues in liver by liquid chromatography tandem mass spectrometry

    • 摘要: 建立了呋喃唑酮代谢物AOZ、呋喃西林代谢物SEM尧、呋喃妥因代谢物AHD、呋喃它酮代谢物AMOZ 的高效液相色谱-串联质谱(HPLC-MS/MS)测定方法、样品经乙酸乙酯提取后,用Oasis HLB 固相萃取柱净化,以乙腈和甲酸-乙酸铵缓冲溶液为流动相,梯度洗脱,采用电喷雾正离子(ESI+)电离,多反应监测(MRM)模式检测,外标法定量。4种硝基呋喃类代谢物在0.5~20.0 ng/mL范围内均具有良好的线性关系,相关系数不低于0.9906,平均加标回收率为91.0%~101.5%,相对标准偏差均小于8%。该方法具有准确、灵敏、高效、环保,适用于猪肝中多种硝基呋喃类代谢物的同时测定。

       

      Abstract: A HPLC-MS/MS method was developed for determination of 4 nitrofuran metabolite residues in liver. The sample was extracted with ethyl acetate and purified by Oasis HLB solid -phase extraction column, then detected by high performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS). Acetonitrile and formic acid-ammonium acetate buffer were used as mobile phase by gradient elution. The analysis of target compounds was carried out by HPLC-MS/MS under positive electrospray ionization (ESI+) and multiple reaction monitoring (MRM) mode. The calibration curves for 4 nitrofuran metabolite residues all had good linear relationships with correlation coefficients not less than 0.9906. The spiked recoveries were ranged from 91.0% to 101.5% with relative standard deviations less than 8%. It was an effective method which fit for the nitrofuran metabolite residues analysis and has high accuracy, precision and sensitivity.

       

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