固相萃取-超高效液相色谱-串联质谱法测定鸡蛋中甲硝唑残留

Determination of metronidazole residues in eggs by solid phase extraction-ultra performance liquid chromatography- tandem mass spectrometry

中文关键词:  甲硝唑  固相萃取  超高效液相色谱-串联质谱法  鸡蛋

英文关键词:metronidazole  solid phase extraction  ultra performance liquid chromatography-tandem mass spectrometry  eggs

中文摘要:

      目的 优化固相萃取-超高效液相色谱-串联质谱法(solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry, SPE-UPLC-MS/MS)测定鸡蛋中甲硝唑残留的分析方法。方法 样品经乙酸乙酯提取, 用MCX固相萃取小柱净化, 以C18色谱柱进行分离, 以0.1%甲酸水-0.1%甲酸甲醇溶液为流动相梯度洗脱分离, 在电喷雾离子源(electrospray ionization, ESI)正离子模式下, 采用多反应监测模式进行定性分析, 以内标法进行定量分析。结果 方法检出限(limit of detection, LOD)和定量限(limit of quantitation, LOQ)分别为0.04 μg/kg和0.2 μg/kg, 回收率为92%~120%, 相对标准偏差为2.33%~8.91%, 精密度较好。在1.00~100.00 μg/L范围内, 甲硝唑的质量浓度与峰面积呈现出良好的线性关系, 其相关系数为0.9996。结论 本方法简单、准确、可靠, 能满足鸡蛋中氯霉素残留分析的要求。

英文摘要:

      Objective To optimize the analytical method for determination of metronidazole residues in eggs by solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry (SPE-UPLC-MS/MS). Methods The samples were extracted with ethyl acetate and purified by MCX solid-phase extraction column. The separation was performed on a C18 column using 0.1% formic acid water-0.1% formic acid methanol solution as the mobile phase gradient elution. Qualitative analysis was performed using multi-reaction monitoring mode in positive ion mode of ESI ion source by electrospray ionization, and quantitative analysis was performed using internal standard method. Results The limit of detection (LOD) and limit of quantitation (LOQ) of the method was 0.04 μg/kg and 0.2 μg/kg, and the recoveries were 92%?120%, relative standard deviations were 2.33%?8.91% respectively. The precision was good. A good linear relationship was established between the mass concentration of metronidazole and the peak area within the range of 1.00?100.00 μg/L, and the correlation coefficient was 0.9996. Conclusion This method is simple, accurate and reliable, and can meet the requirements of metronidazole residue in eggs analysis.