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

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0.33μg/kg和1μg/kg,高氯酸盐在1～10μg/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。

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 0.33μg/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.