固相萃取-高效液相色谱-串联质谱法测定蜂蜜中高氯酸盐
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。
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.
标题：固相萃取-高效液相色谱-串联质谱法测定蜂蜜中高氯酸盐
英文标题：Determination of perchlorate in honey using solid-phase extraction-high performance liquid chromatography-tandem mass spectrometry
作者：
杨志伟 秦皇岛出入境检验检疫局检验检疫技术中心
刘晓茂 秦皇岛出入境检验检疫局检验检疫技术中心
裴岗 秦皇岛出入境检验检疫局检验检疫技术中心
李响 秦皇岛出入境检验检疫局检验检疫技术中心
崔宗岩 秦皇岛出入境检验检疫局检验检疫技术中心
张进杰 秦皇岛出入境检验检疫局检验检疫技术中心
李学民 秦皇岛出入境检验检疫局检验检疫技术中心
曹彦忠 秦皇岛出入境检验检疫局检验检疫技术中心
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,
发表日期：2019-01-08
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