固相萃取-高效液相色谱-串联质谱法测定蜂蜜中高氯酸盐

Determination of perchlorate in honey using solid-phase extraction-high performance liquid chromatography-tandem mass spectrometry

中文关键词:  高效液相色谱-串联质谱法  固相萃取  高氯酸盐  蜂蜜

英文关键词:high performance liquid chromatography-tandem mass spectrometry  solid-phase extraction  perchlorate  honey

中文摘要:

      目的 建立一种固相萃取-高效液相色谱-串联质谱法测定蜂蜜中高氯酸盐的含量。方法 样品用酸化甲醇水提取, WAX固相萃取柱净化, 经Phenyl-hexyl色谱柱分离, 以电喷雾离子源在负离子多反应监测模式下进行测定, 内标法定量。结果 高氯酸盐的检出限和定量限分别为0.33 μg/kg和1 μg/kg, 高氯酸盐在1~ 10 μg/kg的加标水平内的回收率为91.6%~108.3%, 相对标准偏差为2.81%~3.47%。结论 该方法准确、灵敏, 适用于蜂蜜中高氯酸盐的测定。

英文摘要:

      Objective To establish a method for determination of perchlorate in honey by solid-phase extraction-high performance liquid chromatography-tandem mass spectrometry. Methods The samples were extracted with acidified methanol water, purified by WAX solid phase extraction column, separated by phenyl-hexyl chromatographic column, determined by electrospray ion source in the mode of anion multi-reaction monitoring, and quantified by internal standard method determination. Results The limit of detection for perchlorate was 0.33 μg/kg , and the limit of quantitation was 1 μg/kg. The recoveries of perchlorate were 91.6%-108.3% in the range of 1-10 μg/kg, with relative standard deviations of 2.81%-3.47%. Conclusion The method is accurate and sensitive, which is suitable for the determination of perchlorate in honey.