Salting‐out homogeneous liquid‐liquid microextraction for the determination of azole drugs in human urine: Validation using total error concept

Abstract

A salting-out homogeneous liquid-liquid microextraction was proposed for the quantification of four azole drugs in human urine prior to high-performance liquid chromatography analysis. The procedure involved the mixing of the sample with acetonitrile in appropriate volumes followed by the addition of sodium sulfate solution in order to facilitate phase separation. The parameters influencing the extraction performance were studied and optimized using a two-step experimental design. The analytical procedure was thoroughly validated using the accuracy profiles as a graphical decision-making tool.The β-expectation tolerance intervals did not exceed the acceptance criteria of ±15% meaning that 95% of future results will be included in the defined bias limits. The limits of detection of the procedure were satisfactory, ranging between 0.01 and 0.03 μg/mL. The mean analytical bias in the spiking levels was satisfactory and ranged between -10.3 and 4.2% while the relative standard deviation was lower than 5.6%. Monte-Carlo simulations followed by capability analysis were employed to investigate the ruggedness of the sample preparation protocol. The developed method offers advantages compared to previously reported approaches for the same type of analysis including extraction efficiency and scaling down of the sample volume and extraction time.

Salt-Induced Homogeneous Liquid–Liquid Microextraction of Piroxicam and Meloxicam from Human Urine Prior to Their Determination by HPLC-DAD

“…However, the addition of magnesium sulfate and zinc sulfate in the salt solution resulted in an organic upper layer that contained a high water amount and was almost twice its initial volume. This phenomenon has also been reported elsewhere [19], and it can be attributed to the simultaneous extraction of polar interferences that could result in a significant matrix effect. Based on these results, both zinc sulfate and magnesium sulfate were excluded from the consequent trials.…”

“…Typical examples of green extraction techniques used for the determination of drugs in biological matrices include sorbent-based approaches such as solid-phase microextraction [11], fabric phase sorptive extraction (FPSE) [12], capsule phase microextraction (CPME) [13], magnetic solid-phase extraction (MSPE) [14], stir bar sorptive extraction (SBSE) [15], pipette tip-based microextraction [16] and liquid-based approaches such as dispersive liquid-liquid microextraction (DLLME) [17], electromembrane extraction (EME) [18], homogeneous liquid-liquid microextraction (HLLME), etc. [19]. The advances in sample preparation techniques for bioanalytical purposes has recently been reviewed [20].…”

“…Due to its inherent benefits, SI-HLLME has established itself as a useful bioanalytical tool. Typical applications of SI-HLLME include the extraction of azole antimicrobial drugs [19], amphetamines [26], fluoroquinolones [27], antiepileptic drugs [28], amantadine [29], etc. It is noteworthy that HLLME is also in good agreement with some principles of green sample preparation (GSP) that promotes the minimization of waste generation and energy demand, the achievement of high sample throughput and the miniaturization and simplification of the analytical procedure [30].…”

A simple and green liquid chromatography method for the determination of ibuprofen in milk‐containing simulated gastrointestinal media for monitoring the dissolution studies of three‐dimensional‐printed formulations

“…The validation of the proposed UHPLC‐PDA method was performed according to the “ Société française des sciences et techniques pharmaceutiques ” Commission proposal by implementing the accuracy profiles (total‐error concept). The theory behind the accuracy profiles is described in the Supporting Information [21, 22]. For this purpose, two parallel sets of standard solutions (i.e., calibration standards and validation standards) were prepared.…”

Determination of 2,4‐dichlorophenoxyacetic acid in environmental and food samples using salt‐assisted liquid‐liquid extraction coupled with micro‐channel and high‐performance liquid chromatography

“…Salting-out is a sample preparation technique used to separate organic compounds from the aqueous solution by increasing the ionic strength of the aqueous solution [37]. Sodium chloride is a neutral salt most commonly used as a salting-out agent in the SALLE procedure.…”