贺巍巍,杨杰,王雨昕,李雨哲,陈达炜,赵云峰,周爽,方从容.超高效液相色谱-串联质谱法测定食品中高氯酸盐[J].中国食品卫生杂志,2017,29(4):438-444. 本文二维码信息
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超高效液相色谱-串联质谱法测定食品中高氯酸盐
Determination of perchlorate in food by ultra performance liquid chromatography-tandem mass spectrometry
投稿时间:2017-05-04  
DOI:
中文关键词:  超高效液相色谱-串联质谱法  高氯酸盐  食品污染物  食品安全  检测方法
Key Words:Ultra performance liquid chromatography-tandem mass spectrometry  perchlorate  food contaminants  food safety  testing methods
基金项目:国家自然科学基金(21537001);国家食品安全风险评估中心高层次人才队伍建设523项目(1311613106702)
作者单位E-mail
贺巍巍 国家食品安全风险评估中心 卫生部食品安全风险评估重点实验室,北京 100021 heweiwei@cfsa.net.cn,fangcr@cfsa.net.cn 
杨杰 国家食品安全风险评估中心 卫生部食品安全风险评估重点实验室,北京 100021  
王雨昕 国家食品安全风险评估中心 卫生部食品安全风险评估重点实验室,北京 100021  
李雨哲 国家食品安全风险评估中心 卫生部食品安全风险评估重点实验室,北京 100021  
陈达炜 国家食品安全风险评估中心 卫生部食品安全风险评估重点实验室,北京 100021  
赵云峰 国家食品安全风险评估中心 卫生部食品安全风险评估重点实验室,北京 100021  
周爽 国家食品安全风险评估中心 卫生部食品安全风险评估重点实验室,北京 100021  
方从容 国家食品安全风险评估中心 卫生部食品安全风险评估重点实验室,北京 100021 heweiwei@cfsa.net.cn,fangcr@cfsa.net.cn 
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中文摘要:
      目的 建立食品中高氯酸盐的超高效液相色谱-串联质谱(UPLC-MS/MS)的测定方法。方法 香辛料调味品用水提取,蔬菜、水果用乙腈-水(1∶1,V/V)提取,肉、禽、蛋、奶和水产品用乙腈-水(2∶1,V/V)提取,C18柱(3 ml,200 mg)净化,以高氯酸根为内标定量,采用UPLC-MS/MS法测定。结果 在0.3~20.0 μg/L范围内,3种提取溶液中高氯酸盐有良好的线性关系,R2≥0.999。加标浓度在2.0~50.0 μg/kg范围内,内标相对平均回收率为82.6%~108.6%,相对标准偏差(RSD)为1.0%~9.9%。牛奶的定量限为2.0 μg/kg,其他食品的定量限为10.0 μg/kg。结论 本方法简单快捷,定量准确,适用于食品中高氯酸盐的测定。
Abstract:
      Objective To establish a method for the determination of perchlorate in food by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). Methods The perchlorate residue in spices and condiments was extracted with water, that in vegetables and fruits was extracted with acetonitrile-water (1∶1, V/V), and that in meat, poultry, eggs, milk and aquatic products was extracted with acetonitrile-water (2∶1, V/V). The supernatant was cleaned up with C18 SPE (3 ml, 200 mg), and the detection was carried out by UPLC-MS/MS with internal standardmethod for quantification. Results The calibration curve was linear in the concentration range of 0.3-20.0 μg/L (R2≥0.999), the recovery was in the range of 82.6%-108.6%, the relative standard deviation (RSD) was in the range of 1.0%-9.9%, and the limit of detection was 2.0 μg/kg for milk, and 10.0 μg/kg for other food. Conclusion The method was simple, accurate and highly sensitive, and suitable for the determination of perchlorate in food.
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