马妍,陈頔,陈曦,刘婷婷,李琴.分散固相萃取-分散液液微萃取-气相色谱-质谱联用法测定中草药类保健食品中29种有机磷农药残留[J].中国食品卫生杂志,2017,29(5):556-560. 本文二维码信息
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分散固相萃取-分散液液微萃取-气相色谱-质谱联用法测定中草药类保健食品中29种有机磷农药残留
Determination of 29 organophosphorus pesticide residues in health food from Chinese herbal medicines by dispersive solid phase extraction and dispersive liquid-liquid microextraction coupled with gas chromatography-mass spectrometry
投稿时间:2017-06-23  
DOI:
中文关键词:  分散固相萃取  分散液液微萃取  气相色谱-质谱  有机磷农药  保健食品  中草药  食品污染物  测定
Key Words:Dispersive solid phase extraction  dispersive liquid-liquid microextraction  gas chromatography-mass spectrometry  organophosphorus pesticides  health food  Chinese herbal medicine  food contaminants  determination
基金项目:国家自然科学基金青年科学基金资助项目(31400097)
作者单位E-mail
马妍 中国疾病预防控制中心营养与健康所 卫计委微量元素营养重点实验室,北京 100050 mayan_556@163.com,liqin529luck@163.com 
陈頔 中国疾病预防控制中心营养与健康所 卫计委微量元素营养重点实验室,北京 100050  
陈曦 中国疾病预防控制中心营养与健康所 卫计委微量元素营养重点实验室,北京 100050  
刘婷婷 中国疾病预防控制中心营养与健康所 卫计委微量元素营养重点实验室,北京 100050  
李琴 中国环境科学研究院 环境基准与风险评估国家重点实验室,北京 100012
中国环境科学研究院环境标准研究所,北京 100012 
mayan_556@163.com,liqin529luck@163.com 
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中文摘要:
      目的 建立测定中草药类保健食品中有机磷农药残留的分散固相萃取-分散液液微萃取-气相色谱-质谱联用法。方法 样品经含0.5%甲酸的乙腈超声提取,上清液经含无水硫酸镁、N-丙基乙二胺(PSA)、C18的分散固相萃取管(d-SPE)净化后,采用分散液液微萃取(DLLME)步骤,用氯仿萃取、浓缩目标化合物。结果 在最优条件下,线性范围为0.05~1.00 μg/ml,线性相关系数在0.999以上,检出限(LOD)为0.3~3.0 μg/kg,29种有机磷农药的平均加标回收率在70.3%~107.5%之间,相对标准偏差均<10%。结论 该方法具有简便快速、准确灵敏、萃取效率高等特点,可用于中草药类保健食品中有机磷农药残留的检测。
Abstract:
      Objective To establish a method for the determination of pesticide residues in health food made from Chinese herbal medicines by dispersive solid phase extraction and dispersive liquid-liquid microextraction coupled with gas chromatography-mass spectrometry. Methods The samples were ultrasonic extracted by acetonitrile containing 0.5% formic acid. The supernatant was purified by dispersive solid phase extraction (d-SPE) extraction tube with anhydrous magnesium sulfate, N-propyl ethylenediamine (PSA) and C18, and then the target compounds were extracted and concentrated by the method of dispersive liquid-liquid microextraction (DLLME). Results Under optimal conditions, the linear range was 0.05-1.00 μg/ml, the linear correlation coefficient was above 0.999, the limit of detection was 0.3-3.0 μg/kg, the average recoveries of 29 kinds of pesticides were between 70.3% and 107.5%, and the relative standard deviation was less than 10%. Conclusion The method was simple, rapid, accurate and sensitive, and it could be used for the detection of organophosphorus pesticide residues in health food made from Chinese herbal medicines.
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