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食品研究与开发:2013,34(18):-
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含油脂食品中16种邻苯二甲酸酯测定的前处理方法研究
王亚琴,祝红昆,冯雷,牛之瑞,珠娜,张晓红
(云南省产品质量监督检验研究院 云南 昆明650023,云南省产品质量监督检验研究院,云南省产品质量监督检验研究院 云南 昆明650023,云南省产品质量监督检验研究院 云南 昆明650023,云南省产品质量监督检验研究院 云南 昆明650023,云南省产品质量监督检验研究院 云南 昆明650023)
Research on the sample pretreatment methods of Phthalic Acid Esters in FoodContaining Fat
WANG Yaqin,zhu hong kun,FENG Lei,NIU Zhiriu,ZHU Na and ZHANG Xiaohong
(Yunnan Institute of Product Quality Supervision and Inspection,Yunnan Institute of Product Quality Supervision and Inspection,Yunnan Institute of Product Quality Supervision and Inspection,Yunnan Institute of Product Quality Supervision and Inspection,Yunnan Institute of Product Quality Supervision and Inspection,Yunnan Institute of Product Quality Supervision and Inspection)
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投稿时间:2013-06-08    修订日期:2013-09-04
中文摘要: 建立了同时检测含油脂食品中16种邻苯二甲酸酯类化合物的分散固相萃取-气相色谱-质谱(GC- MS) 分析方法。样品经正己烷饱和的乙腈提取,提取液通过PSA填料进行分散固相萃取净化,定性和定量选择离子监测模式(SIM)测定。结果表明,含油脂食品中16 种邻苯二甲酸酯的在50和100 ug/kg添加水平下的加标回收率为66.81%~101.55%,相对标准偏差3.72~9.6%。方法灵敏度、精密度和检出限都能满足日常检测分析的要求,简便、快速、准确,避免了含油脂食品使用凝胶色谱仪这一传统方法大量使用有机溶剂的弊端,节约了检测成本,提高了工作效率。更重要的是,最大限度的减小前处理过程实验仪器、试剂带入的PAEs干扰,使检测结果更准确。
Abstract:A method for the simultaneous determination of 16 phthalate esters in food Containing Fat by Dispersive Solid Phase Extraction- Gas Chromatography-Mass Spectrometry ( d- SPE- GC- MS) was developed and evaluated. The samples were extracted with acetonitrile(saturated with hexane), and the extract was cleaned up by PSA d- SPE. The qualitative and quantitative analysis were used with SIM mode.The results showed that the average recoveries rate were in the range of 66.81%~101.55% at the spiked levels of 50 and 100 ug /kg; and the RSDs of precision were 3.72~9.6%.Precision,Sensitivity and Detection Limit meet the challenge of analysis. The method is simple,rapid,and accurate,which can improve work efficiency and reduce the cost.It can avoid the the large solvent consumption in the Usage of gel permeation chromatography.More importantly, disturbance of Instrument and reagent in experiment were decreased to a minimum.
keywords: GC- MS  PAEs  Food Containing Fat
文章编号:QY20130143     中图分类号:    文献标志码:
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