Determination of Non-Steroidal Anti-Inflammatory Drugs in Human Urine Sample using HPLC/UV and Three Phase Hollow Fiber-Liquid Phase Microextraction (HF-LPME)

Abstract

Three phase hollow fiber-liquid phase microextraction (HF-LPME), which is faster, simpler and uses a more environmentally friendly sample-preparation technique, was developed for the analysis of Non-Steroidal AntiInflammatory Drugs (NSAIDs) in human urine. For the effective simultaneous extraction/concentration of NSAIDs by three phase HF-LPME, parameters (such as extraction organic solvent, pH of donor/acceptor phase, stirring speed, salting-out effect, sample temperature, and extraction time) which influence the extraction efficiency were optimized. NSAIDs were extracted and concentrated from 4 mL of aqueous solution at pH 3 (donor phase) into dihexyl ether immobilized in the wall pores of a porous hollow fiber, and then extracted into the acceptor phase at pH 13 located in the lumen of the hollow fiber. After the extraction, 5 µL of the acceptor phase was directly injected into the HPLC/UV system. Simultaneous chromatographic separation of seven NSAIDs was achieved on an Eclipse XDB-C18 (4.6 mm i.d. × 150 mm length, 5 µm particle size) column using isocratic elution with 0.1% formic acid and methanol (30:70) at a HPLC-UV/Vis system. Under optimized conditions (extraction solvent, dihexyl ether; pH donor , 3; pH acceptor , 13; stirring speed, 1500 rpm; NaCl salt, 10%; sample temperature, 60 o C; and extraction time, 45 min), enrichment factors (EF) were between 59 and 260. The limit of detection (LOD) and limit of quantitation (LOQ) in the spiked urine matrix were in the concentration range of 5-15 ng/mL and 15-45 ng/mL, respectively. The relative recovery and precision obtained were between 58 and 136% and below 15.7% RSD, respectively. The calibration curve was linear within the range of 0.015-0.96 ng/mL with the square of the correlation coefficient being more than 0.997. The established method can be used to analyse of NSAIDs of low concentration (ng/mL) in urine.

Microextraction by packed sorbent and HPLC–PDA quantification of multiple anti-inflammatory drugs and fluoroquinolones in human plasma and urine

“…provide a better transfer of acid drugs into the organic phase 23 , thus improving the performance of extraction.…”

Determination of Non‐Steroidal Anti‐Inflammatory Drugs in Urine by HPLC–UV/Vis Analysis Coupled with Electromembrane Extraction

“…Determination of NSAIDs in aqueous matrices has been attempted using chromatographic methods such as gas chromatography (GC), gas chromatography/mass spectrometry (GC/MS), high‐performance liquid chromatography (HPLC), and liquid chromatography/mass spectrometry (LC/MS) . Moreover, various sample preparation methods have been investigated, with most of them based on traditional solid‐phase extraction (SPE) and liquid–liquid extraction (LLE) techniques.…”

“…Determination of NSAIDs in aqueous matrices has been attempted using chromatographic methods such as gas chromatography (GC), gas chromatography/mass spectrometry (GC/MS), high-performance liquid chromatography (HPLC), and liquid chromatography/mass spectrometry (LC/MS). [4][5][6][7] Moreover, various sample preparation methods have been investigated, with most of them based on traditional solid-phase extraction (SPE) and liquidliquid extraction (LLE) techniques. However, SPE methods utilize costly disposable SPE cartridges and require large volumes of organic solvents to condition/wash these cartridges and extract analytes, whereas LLE consumes large amounts of samples and organic extraction solvents, additionally suffering from long sample preparation times.…”

Simultaneous Determination of Nonsteroidal Anti‐Inflammatory Drugs in Aqueous Samples Using Dispersive Liquid–Liquid Microextraction and HPLC Analysis

“…Currently the pursuit of “green chemistry” with precise, accurate, simple, fast, and environmentally friendly methods is desirable. SPME is a representative microextraction method that requires no organic solvents and uses a simple, time‐saving sample preparation, however SPME encounters problems related to robustness and reproducibility due to spoilage of the fibers and low extraction efficiencies, and uses expensive expendable solid‐phase cartridges . Liquid‐phase microextraction (LPME) methods include single‐drop microextraction (SDME), hollow‐fiber liquid‐phase microextraction (HF‐LPME), and dispersive liquid–liquid microextraction (DLLME) .…”

“…SPME is a representative microextraction method that requires no organic solvents and uses a simple, time-saving sample preparation, however SPME encounters problems related to robustness and reproducibility due to spoilage of the fibers and low extraction efficiencies, and uses expensive expendable solid-phase cartridges. 11,12 Liquid-phase microextraction (LPME) methods include single-drop microextraction (SDME), 13 hollowfiber liquid-phase microextraction (HF-LPME), and dispersive liquid-liquid microextraction (DLLME). 14,15 These methods use a small amount (microliters) of organic solvent and provide good extraction recovery and concentration effects.…”