柱切换在线前处理法鉴别地沟油的离子色谱研究

doi:10.3785/j.issn.1008-9497.2016.02.017

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摘要建立了同时检测食用油及地沟油中的无机阴离子(F^-、Cl^-、SO₄^2-)和有机酸(CH₃CO₂^-、CHO₂^-)的离子色谱柱切换在线前处理方法.采用一根NG1反相色谱柱作为前处理柱在线去除样品中的水溶性有机基质,通过柱切换技术,由淋洗液将柱内富集的离子带至阴离子分析柱中分离,从而达到在线前处理的目的.在优化的色谱条件下,被分析离子浓度在0.05~10 mg·L^-1时,线性相关系数均大于0.9990;进样量25 μL,方法的检出限为4~41 μg·L^-1(信噪比S/N=3);加标回收率在75.6%~87.7%;相对标准偏差在0.85%~2.34%(n=6);实验结果表明,地沟油中甲酸和乙酸的含量明显高于食用油.本方法对食用油和地沟油的鉴别具有较好的实用价值,适用于食用油及地沟油中常规阴离子和有机酸的同步检测,具有快速、灵敏、选择性好等优点.

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	赵训燕
	倪承珠
	朱彬和
	张培敏
	张嘉捷
	陈素清
	朱岩

关键词 ：离子色谱, 柱切换, 常规阴离子, 有机酸

Abstract：The ion chromatography with on-line sample pretreatment using column-switching technique is applied to the simultaneous analysis of the conventional inorganic anions and organic acids in edible oils and illegal cooking oils. In this work, a polymer-based reversed-phase column was used as the pretreatment column. Via column-switching technique, sample solution with target ions were eluted from a collection loop to the analytical columns with matrix eliminated on-line. A series of standard solutions consisting of target ions of various concentrations from 0.05 to 10 mg·L^-1 are analyzed, with a correlation coefficient r≥0.9990 and a satisfactory repeatability (RSD≤2.34%, n=6). The limits of detection are in the range from 4 to 41 μg·L^-1 based on S/N of 3 and the 25 μL injection volume. The average spiked recovery rates are between 75.6% and 87.7%. The result shows that the concentration of acetate and formate are significantly higher in the illegal cooking oils than edible oils. The on-line sample pretreatment IC system is convenient and practical for the determination of conventional inorganic anions and organic acids in edible and illegal cooking oil samples.

Key words： ion chromatography column-switching conventional inorganic anions organic acids

收稿日期: 2015-06-23

基金资助:国家重大科学仪器设备开发专项(2012YQ09022903);浙江省自然科学基金资助项目(Y12B050014,LQ13B050001,LY12B05003).

通讯作者: 朱岩,E-mail:zhuyan@zju.edu.cn. E-mail: zhuyan@zju.edu.cn

作者简介: 赵训燕(1991-),ORCID:http://orcid.org/0000-0002-9731-991X,女,硕士研究生,主要从事离子色谱研究.

引用本文:

赵训燕, 倪承珠, 朱彬和, 张培敏, 张嘉捷, 陈素清, 朱岩. 柱切换在线前处理法鉴别地沟油的离子色谱研究[J]. 浙江大学学报（理学版）, 2016, 43(2): 220-225.
ZHAO Xunyan, NI Chengzhu, ZHU Binhe, ZHANG Peimin, ZHANG Jiajie, CHEN Suqing, ZHU Yan. Distinguishing illegal cooking oils by ion chromatography with column-switching on-line sample pretreatment. Journal of ZheJIang University(Science Edition), 2016, 43(2): 220-225.

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http://www.journals.zju.edu.cn/sci/CN/10.3785/j.issn.1008-9497.2016.02.017 或 http://www.journals.zju.edu.cn/sci/CN/Y2016/V43/I2/220

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