色谱

色谱 ›› 2013, Vol. 31 ›› Issue (9): 825-830.DOI: 10.3724/SP.J.1123.2013.03002

• 研究论文 • 上一篇    下一篇

一种亲水-亲油复合固相萃取填料的制备及其在食品安全检测中的应用

包建民1,2, 谢丹1,2, 孙超慧1, 李优鑫1, 王俊菊3   

  1. 1. 天津市现代药物传递及功能高效化重点实验室, 天津大学药物科学与技术学院, 天津 300072;
    2. 天津奥顺达科技有限公司, 天津 300452;
    3. 天津市兽药饲料监察所, 天津 300402
  • 收稿日期:2013-03-01 修回日期:2013-05-03 出版日期:2013-09-28 发布日期:2013-09-02
  • 通讯作者: 李优鑫
  • 基金资助:

    国家自然科学基金项目(21075088);天津大学自主创新基金项目(1102213).

Preparation of a hydrophilic-lipophilic composite solid phase extraction material and application in food safety inspection

BAO James Jianmin1,2, XIE Dan1,2, SUN Chaohui1, LI Youxin1, WANG Junju3   

  1. 1. Tianjin Key Laboratory for Modern Drug Delivery & High-Efficiency, School of Pharmaceutical Science and Technology, Tianjin University, Tianjin 300072, China;
    2. Tianjin ASD Scientific Co., Ltd., Tianjin 300452, China;
    3. Tianjin Institute of Veterinary Drugs and Feed Control, Tianjin 300402, China
  • Received:2013-03-01 Revised:2013-05-03 Online:2013-09-28 Published:2013-09-02

PDF

195

被引次数

13

摘要：

合成了一种以二乙烯苯和N-乙烯吡咯烷酮为单体的高分子聚合物固相萃取填料(DVB-NVP),以6种不同极性的化合物为模型化合物,结合高效液相色谱法(HPLC)对该填料进行了系统的评价,并与传统的C18填料及商品化同类型填料做对比;对填料进行了磺酸化修饰(DVB-NVP-SO3H),并将合成的填料应用于复杂基质中化合物的分析。结果表明:该填料对不同极性化合物的回收率在95.55%~101.08%之间,优于商品化C18填料,与商品化同类型填料相当。DVB-NVP对于白酒中邻苯二甲酸二甲酯、邻苯二甲酸二乙酯、邻苯二甲酸二丁酯的分析回收率分别为102.55%、102.99%、102.11%,相对标准偏差分别为2.11%、1.69%、0.79%; DVB-NVP-SO3H用于对猪肉中的可乐定和赛庚啶进行分析,回收率分别为89.23%和91.42%,相对标准偏差分别为8.21%和8.86%,符合生物样品分析要求。所合成的填料具有普适性,并具有较高的回收率,应用前景广泛。

关键词: 高效液相色谱法, 固相萃取, 可乐定, 强阳离子交换填料, 亲水-亲油平衡, 赛庚啶, 食品安全检测, 塑化剂

Abstract:

A copolymer of divinylbenzene and N-vinyl pyrrolidone (DVB-NVP) was synthesized for the purpose of solid phase extraction (SPE). Its performance as an SPE resin was evaluated using six model compounds having different polarities. Aqueous samples containing those compounds were applied to SPE cartridges containing the aforementioned copolymer as well as the classic C18 and Oasis HLB for comparison, and the SPE processed samples were analyzed by using high performance liquid chromatography (HPLC) for quantitation. Then, the copolymer DVB-NVP was sulfonated to modify the surface properties. The surface modified materials were used to analyse complex samples. The results showed that DVB-NVP had high recoveries for the six compounds ranging from 95.55% to 101.08% which were better than those of the C18 and were comparable to those of Oasis HLB. In applying to real samples, the recoveries for dimethyl phthalate, diethyl phthalate and dibutyl phthalate in liquor were 102.55%, 102.99% and 102.11%, with the RSDs of 2.11%, 1.69%, 0.79% respectively. Similarly, the recoveries for clonidine and cyproheptadine in pork were 89.23% and 91.42% with the RSDs of 8.21% and 8.86%, respectively.

Key words: clonidine, cyproheptadine, food safety inspection, high performance liquid chromatography (HPLC), hydrophilic-lipophilic balance, plasticizers, solid phase extraction (SPE), strong cation exchange packing

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