高效液相色谱-串联质谱法测定豆芽中的甲硝唑和羟基甲硝唑

Determination of metronidazole and hydroxymetronidazole in bean sprouts by high performance liquid chromatography-tandem mass spectrometry

中文关键词:  豆芽  甲硝唑  羟基甲硝唑  高效液相色谱-串联质谱法

英文关键词:bean sprouts  metronidazole  hydroxymetronidazole  high performance liquid chromate graphy-tandem mass spectrometry

中文摘要:

      目的 建立高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry, HPLC-MS/MS)测定豆芽中甲硝唑和羟基甲硝唑检测方法。方法 样品经乙酸乙酯提取2次, 旋转蒸发, 混合阳离子交换柱净化, 经InfinityLabPoroshell SB-Aq色谱柱分离, HPLC-MS/MS检测, 内标法定量分析。结果 甲硝唑和羟基甲硝唑在1.0～100.0 ?g/L范围内线性关系良好, 线性相关系数均大于0.998。在1.0、5.0和10.0 ?g/kg 3个添加水平下的平均回收率为83%～105%, 相对标准偏差在2.2%～5.5%之间, 检出限为0.3 ?g/kg, 定量限为1.0 ?g/kg。结论 该方法灵敏可靠, 回收率稳定, 适用于豆芽中甲硝唑和羟基甲硝唑的同时测定。

英文摘要:

      Objective To establish a methodfor the determination of metronidazole andhydroxymetronidazole in bean sproutsbyhigh performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS). Methods The sample was extracted twice with ethyl acetate, rotary evaporated, purified by a mixed cation exchange column, separated by an InfinityLabPoroshell SB-Aq column, detected by HPLC-MS/MS, and quantitatively analyzed by internal standard method. Results Metronidazole and hydroxymetronidazole had good linear relationships in the range of 1.0?100.0?g/L, and the linear correlation coefficients were both greater than 0.998. The average recoveries at spiked levels of 1.0, 5.0 and 10.0 μg/kg ranged from 83%?105%, with relative standard deviations (RSD) from 2.2% to 5.5%. The limit of detectionand limit of quantification were 0.3 ?g/kg and 1.0 ?g/kg, respectively. Conclusion This method is sensitive and accurate, and has stable recovery rate, which is suitable for simultaneous determination of metronidazole and hydroxymetronidazole in bean sprout.