Tandem-Column High Performance Liquid Chromatography Separation of Non-Steroidal Anti-Inflammatory Drugs (NSAIDs)

IF 1.2 4区化学 Q4 BIOCHEMICAL RESEARCH METHODS

Chromatographia Pub Date : 2023-10-27 DOI:10.1007/s10337-023-04286-9

Megan E. Marrazzo, Joe P. Foley

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Abstract

A tandem-column liquid chromatographic method was developed to separate ten non-steroidal anti-inflammatory drugs (Aceclofenac, Aspirin, Carprofen, Celecoxib, Diclofenac, Flurbiprofen, Ibuprofen, Ketoprofen, Naproxen, Salicylic Acid) using an achiral tandem-column configuration under reversed-phase conditions. An NSAID test mix was prepared with 0.5 mg/mL thiourea as a t₀ marker and 0.5 mg/mL of the above NSAIDs in 1:1 acetonitrile: 0.2% formic acid. Three different 5-cm columns were investigated individually and in two different tandem-column configurations: an octyl (C8) column, a perfluorophenyl (PFP) column, and a biphenyl (BP) column. The two tandem configurations investigated were a PFP column followed by either a BP or C8 column. While none of the individual columns provided the selectivity needed to separate two sets of critical pairs (Ketoprofen and Naproxen; Flurbiprofen and Ibuprofen), the unique selectivity provided by the two tandem-column combinations enabled both critical pairs to be separated. The PFP + BP tandem column combination was able to separate the 10 NSAIDs with baseline or greater resolution in less than 25 min.

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串联柱高效液相色谱法分离非甾体抗炎药

开发了一种串联柱液相色谱法，在反相条件下使用非手性串联柱结构分离十种非甾体抗炎药（Aceclofenac、Aspirin、Carprofen、塞来昔布、双氯芬酸、Flurbirofen、布洛芬、酮洛芬、萘普生、水杨酸）。用0.5mg/mL硫脲作为t0标记物和0.5mg/mL上述非甾体抗炎药在1:1乙腈：0.2%甲酸中制备非甾体消炎药测试混合物。分别研究了三种不同的5cm柱，并采用两种不同的串联柱配置：辛基（C8）柱、全氟苯基（PFP）柱和联苯（BP）柱。研究的两种串联结构是PFP柱，然后是BP或C8柱。虽然没有一个单独的柱提供分离两组关键对（酮洛芬和萘普生；氟比洛芬和布洛芬）所需的选择性，但两个串联柱组合提供的独特选择性使两个关键对都能够分离。PFP + BP串联柱组合能够在不到25分钟的时间内以基线或更高的分辨率分离10种非甾体抗炎药。

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来源期刊

Chromatographia 化学-分析化学

CiteScore

3.40

自引率

5.90%

发文量

103

审稿时长

2.2 months

期刊介绍： Separation sciences, in all their various forms such as chromatography, field-flow fractionation, and electrophoresis, provide some of the most powerful techniques in analytical chemistry and are applied within a number of important application areas, including archaeology, biotechnology, clinical, environmental, food, medical, petroleum, pharmaceutical, polymer and biopolymer research. Beyond serving analytical purposes, separation techniques are also used for preparative and process-scale applications. The scope and power of separation sciences is significantly extended by combination with spectroscopic detection methods (e.g., laser-based approaches, nuclear-magnetic resonance, Raman, chemiluminescence) and particularly, mass spectrometry, to create hyphenated techniques. In addition to exciting new developments in chromatography, such as ultra high-pressure systems, multidimensional separations, and high-temperature approaches, there have also been great advances in hybrid methods combining chromatography and electro-based separations, especially on the micro- and nanoscale. Integrated biological procedures (e.g., enzymatic, immunological, receptor-based assays) can also be part of the overall analytical process.