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浙江大学学报(理学版)  2016, Vol. 43 Issue (2): 220-225    DOI: 10.3785/j.issn.1008-9497.2016.02.017
化学     
柱切换在线前处理法鉴别地沟油的离子色谱研究
赵训燕1,2, 倪承珠1,2, 朱彬和1,2, 张培敏1, 张嘉捷1, 陈素清3, 朱岩1,2
1. 浙江大学化学系, 浙江杭州 310028;
2. 浙江大学浙江省微量有毒化学物健康风险评估技术研究重点实验室, 浙江杭州 310028;
3. 台州学院制药与化学工程学院, 浙江台州 317000
Distinguishing illegal cooking oils by ion chromatography with column-switching on-line sample pretreatment
ZHAO Xunyan1,2, NI Chengzhu1,2, ZHU Binhe1,2, ZHANG Peimin1, ZHANG Jiajie1, CHEN Suqing3, ZHU Yan1,2
1. Department of Chemistry, Zhejiang University, Hangzhou 310028, China;
2. Zhejiang Provincial Key Laboratory of Health Risk Appraisal for Trace Toxic Chemicals, Zhejiang University, Hangzhou 310028, China;
3. School of Pharmaceutical and Chemical Engineering, Taizhou University, Taizhou 317000, Zhejiang Province, China
 全文: PDF(989 KB)  
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-、SO42-)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.
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 出版日期: 2016-03-12
CLC:  O657.7  
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.
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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.

链接本文:

https://www.zjujournals.com/sci/CN/10.3785/j.issn.1008-9497.2016.02.017        https://www.zjujournals.com/sci/CN/Y2016/V43/I2/220

[1] 崔晓举,蒋世云,张夏辉,等.地沟油检测技术研究进展[J]. 化学分析计量,2013(2):100-104. CUI Xiaoju, JIANG Shiyun, ZHANG Xiahui, et al. Research progress on detection items of the hogwash oil[J]. Chemical Analysis and Meterage, 2013(2):100-104.
[2] 李沂光,单杨,李高阳,等.地沟油检测方法研究现状与其应用分析[J].食品与机械,2012,28(3):262-265. LI Yiguang, SHAN Yang, LI Gaoyang, et al. Current situation and application analysis of detection methods of illegal cooking oil[J]. Food and Machinery,2012,28(3):262-265.
[3] 王乐,胡建华.食用油掺伪餐饮业废油脂鉴别检测方法研究进展[J].中国油脂,2007,32(9):75-77. WANG Le, HU Jianhua. Advance in discrimination method of edible oil adulterated waste cooking oil[J]. Chinese Grease, 2007,32(9):75-77.
[4] 王立,汪正范.色谱分析样品处理[M].北京:化学工业出版社,2006:3-5. WANG Li, WANG Zhengfan. Sample Processing for Chromatographic Analysis[M]. Beijing:Chemical Industry Press,2006:3-5.
[5] BULDINI P L, FERRI D, SHARMA J L. Determination of some inorganic species in edible vegetable oils and fats by ion chromatography[J]. Journal of Chromatogr A, 1997, 789(1):549-555.
[6] SILVEIRA E L C, CALAND L B, TUBINO M. Simultaneous quantitative analysis of the acetate, formate, chloride, phosphate and sulfate anions in biodiesel by ion chromatography[J]. Fuel,2014,124(15):97-101.
[7] YANG Y, HE J, HUANG Z P, et al. Analysis of hexavalent chromium in colla corii asini with on-line sample pretreatment valve-switching ion chromatography[J]. Journal of Chromatogr A,2013,1305:171-175.
[8] WANG K, LEI Y, EITEL M, et al. Ion chromatographic analysis of anions in ammonium hydroxide, hydrofluoric acid, and slurries, used in semiconductor processing[J]. Journal of Chromatogr A, 2002, 956(1/2):109-120.
[9] VERMEIREN K. Trace anion determination in concentrated hydrofluoric acid solutions by two-dimensional ion chromatography I. Matrix elimination by ion-exclusion chromatography[J]. Journal of Chromatogr A,2005,1085(1):66-73.
[10] 贺婕,余家胜,黄忠平,等.离子色谱柱切换在线前处理法同时测定皮革及织物中的三价铬与六价铬离子[J].分析化学,2014(8):1190-1195. HE Jie, YU Jiasheng. HUANG Zhongping, et al. Simultaneous determination of trivalent and hexavalent chromium in leather and cloth by ion chromatography with the on-line sample pretreatment column-switching technique[J]. Chinese Journal of Analytical Chemistry,2014(8):1190-1195.
[11] STOVER F S. Automated trace anion determinations in concentrated electronic grade phosphoric acid by ion chromatography[J]. Journal of Chromatogr A,2002,956(1/2):121-128.
[12] WANG N, WANG R, ZHU Y. A novel ion chromatography cycling-column-switching system for the determination of low-level chlorate and nitrite in high salt matrices[J]. Journal of Hazardous Materials, 2012,235/236:123-127.
[13] ZHONG Y Y, ZHOU W F, ZHU H B, et al. A single pump column-switching technique coupled with polystyrene-divinylbenzene-carbon nanotubes column for the determination of trace anions in different concentrated organic matrices by ion chromatography[J]. Analytica Chimica Acta,2011,686(1/2):1-8.
[14] 朱作艺,许锦钢,钟乃飞,等.离子色谱阀切换快速测定六氟磷酸根及多种阴离子[J].分析化学,2011(11):1738-1742. ZHU Zuoyi, XU Jingang, ZHONG Naifei, et al. Fast determination of hexafluorophosphate, fluorid, chloride, nitrate and sulfate inorganic anions by ion chromatography with valve switching[J]. Chinese Journal of Analytical Chemistry A,2011(11):1738-1742.
[15] HUANG Z, NI C, WANG F, et al. Simultaneous determination of peroxydisulfate and conventional inorganic anions by ion chromatography with the column-switching technique[J]. Journal of Separation Science,2014,37(3):198-203.
[16] 魏益华,张金艳,戴廷灿,等.离子色谱法测定地沟油和食用油中氯离子含量[J].食品科学, 2011(12):213-215. WEI Yihua, ZHANG Jinyan, DAI Tingcan, et al. Determination of chlorine in hogwash oil and edible oil by ion chromatography[J]. Food Science, 2011(12):213-215
[17] 张咏,李莹,蔡春明.离子色谱法鉴别地沟油的应用研究[J].中国粮油学报, 2012(1):107-110. ZHANG Yong, LI Ying, CAI Chunming. Identification of hogwash oil through ion-chromatogram[J]. Journal of the Chinese Cereals and Oils Association,2012(1):107-110.
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