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离子对色谱法和胶束电动毛细管色谱法在分析人生物体液中的β-肾上腺素能阻滞剂中的应用。

Ion-pair chromatography and micellar electrokinetic capillary chromatography in analyzing beta-adrenergic blocking agents from human biological fluids.

作者信息

Lukkari P, Sirén H

机构信息

Laboratory of Analytical Chemistry, Department of Chemistry, University of Helsinki, Finland.

出版信息

J Chromatogr A. 1995 Nov 24;717(1-2):211-7. doi: 10.1016/0021-9673(95)00488-2.

DOI:10.1016/0021-9673(95)00488-2
PMID:8520676
Abstract

Ion-pair chromatography (IPC) and micellar electrokinetic capillary chromatography (MECC) were used for the separation and determination of parent beta-blockers from human biological fluids. In both these techniques, N-cetyl-N,N,N-trimethylammonium bromide (CTAB) was used as a buffer additive. In IPC, CTAB was an ion-pair former, and in MECC it was a micelle-forming surfactant. The effectiveness of the IPC method using methanol-gradient elution and that of MECC were compared for drug-spiked serum and urine samples. Detection was performed with a diode-array detector in the IPC method and with a 214-nm filter in the MECC technique. In both methods a phosphate buffer (pH 7.0) was used. In MECC the buffer solution contained 10 mM CTAB, while in IPC the CTAB concentration was decreased from 7 to 4 mM during the separation when a methanol gradient was used. The study showed that the IPC technique performed better for bioanalyses than the high-performance MECC technique, since in MECC UV detection presented a problem because of the low sample concentration. However, in MECC sample preparation was less time-consuming, using hydrolyzation and protein precipitation and, unlike the IPC technique, it did not require any liquid-liquid extraction step.

摘要

离子对色谱法(IPC)和胶束电动毛细管色谱法(MECC)被用于从人体生物流体中分离和测定母体β受体阻滞剂。在这两种技术中,溴化十六烷基三甲基铵(CTAB)被用作缓冲添加剂。在离子对色谱法中,CTAB是离子对形成剂,而在胶束电动毛细管色谱法中它是形成胶束的表面活性剂。对加药血清和尿液样本比较了采用甲醇梯度洗脱的离子对色谱法和胶束电动毛细管色谱法的有效性。离子对色谱法采用二极管阵列检测器进行检测,胶束电动毛细管色谱法采用214nm滤光片进行检测。两种方法均使用磷酸盐缓冲液(pH 7.0)。在胶束电动毛细管色谱法中,缓冲溶液含有10mM CTAB,而在离子对色谱法中,使用甲醇梯度时,CTAB浓度在分离过程中从7mM降至4mM。研究表明,离子对色谱技术在生物分析方面比高性能胶束电动毛细管色谱技术表现更好,因为在胶束电动毛细管色谱法中,由于样品浓度低,紫外检测存在问题。然而,在胶束电动毛细管色谱法中,样品制备耗时较少,采用水解和蛋白质沉淀法,并且与离子对色谱技术不同,它不需要任何液-液萃取步骤。

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