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采用分子印迹聚合物纳米粒子结合 HPLC-DAD 检测法测定生物样品中的氟哌啶醇。

Determination of haloperidol in biological samples using molecular imprinted polymer nanoparticles followed by HPLC-DAD detection.

机构信息

Department of Chemistry, Shahid Beheshti University, G.C., Evin, Tehran, Iran.

出版信息

Int J Pharm. 2013 Sep 10;453(2):601-9. doi: 10.1016/j.ijpharm.2013.05.054. Epub 2013 Jun 3.

Abstract

In this study an extraction procedure using molecular imprinted polymer nanoparticles for the determination of haloperidol in biological samples is proposed. The haloperidol imprinted polymer nanoparticles were synthesized successfully by precipitation polymerization in a flask containing haloperidol as a template, ethyleneglycoldimethacrylate as a crosslinking agent, methacrylic acid as a functional monomer, and 2,2'-azobisisobutyronitrile as an initiator. The leached and unleached polymer nanoparticles have been characterized by infrared spectroscopy and scanning electron microscopy. The effect of different variables such as the pH of solution, uptake and elution time, type, and the least amount of eluent for elution of haloperidol from polymer was evaluated. Extraction efficiencies more than 97% were obtained by elution of the polymer with 1.5 mL of methanol-acetic acid-trifluoroacetic acid 79.9:20:0.1. Under optimal conditions maximum adsorption capacity was obtained 153.84 mg g(-1). The detection limit of the proposed procedure was between 0.2 and 0.35 μg L(-1). Finally this method was applied to the determination of haloperidol in plasma and urine samples and satisfactory results were achieved (RSD<6.9%).

摘要

本研究提出了一种使用分子印迹聚合物纳米粒子提取生物样品中氟哌啶醇的方法。氟哌啶醇印迹聚合物纳米粒子通过在含有氟哌啶醇作为模板、乙二醛二甲基丙烯酸酯作为交联剂、甲基丙烯酸作为功能单体和 2,2'-偶氮二异丁腈作为引发剂的烧瓶中沉淀聚合成功合成。已通过红外光谱和扫描电子显微镜对浸出和未浸出的聚合物纳米粒子进行了表征。评估了不同变量的影响,例如溶液的 pH 值、摄取和洗脱时间、类型以及从聚合物中洗脱氟哌啶醇的最少洗脱液量。通过用 1.5 mL 甲醇-乙酸-三氟乙酸 79.9:20:0.1 洗脱,可获得超过 97%的萃取效率。在最佳条件下,最大吸附容量为 153.84 mg g(-1)。该方法的检测限在 0.2 和 0.35 μg L(-1) 之间。最后,该方法应用于血浆和尿液样品中氟哌啶醇的测定,取得了满意的结果(RSD<6.9%)。

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