Determination of psychoactive drugs in serum using conductive vial electromembrane extraction combined with UHPLC-MS/MS

This study is focused on proposing a new design and setup for electromembrane extraction. A new cap was designed and conductive vials of different shapes were fabricated using three‐dimensional printing. The new cap holds three fibers to enhance electromembrane extraction recovery. Conductive vials can simultaneously perform as electrodes therefore, there is no need to include an electrode in sample solutions. Phenobarbital and phenytoin were used as model compounds to assess the setup performance. Under optimal conditions, these analytes were extracted from the sample solution at pH = 9 to the acceptor solution at pH = 13 with a voltage of 40 V for 20 min, while 1‐octanol was employed as the supported‐liquid‐membrane. The influence of conductive vials geometry on the recovery was examined and the effects of different shapes were studied by performing numerical simulation to establish electric potential distribution. Of the vials tested with circular, triangular, and floral‐like cross‐sections the latter exhibited the best voltage distribution. The circular vial had the highest recovery attributed to its better hydrodynamic shape, which allows rapid fluid sample transport and therefore enhanced system recovery. The extraction recovery and relative standard deviation of the circular vial with three fibers were 33.0 and 7.6 for phenobarbital and 42.2 and 10.4 for phenytoin.

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“…In another work, Skaalvik et al. [37] used similar equipment to extract basic lipophilic drugs from serum.…”

Section: Introductionmentioning

confidence: 99%

“…The first commercial equipment for EME, where coupling the electrical potential is through sample and acceptor vials made from a conducting polymer was introduced by Drobnjak et al [36]. In another work, Skaalvik et al [37] used similar equipment to extract basic lipophilic drugs from serum.…”

Section: Introductionmentioning

confidence: 99%

A novel three‐dimensional printed device with conductive elements for electromembrane extraction combined with high‐performance liquid chromatography and ultraviolet detector

Dolatabadi

Mohammadi

Walker

2022

J of Separation Science

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“…EME has been carried out in a number of technical formats based on hollow-fibres, 96-well plates, [9][10][11] and microchip technology. [12][13][14] A commercial EME device based on conductive vials is under development, and prototype equipment has been used in extraction of basic drugs from serum 15 and plasma. 16 Validation data associated with the prototype device were accordance with recommended guidelines for bioanalytical measurements.…”

Section: Introductionmentioning

confidence: 99%

Determination of amphetamine enantiomers in urine by conductive vial electromembrane extraction and ultra‐high performance supercritical fluid chromatography tandem mass spectrometry

Skaalvik

Øiestad

Pedersen‐Bjergaard

et al. 2023

Drug Testing and Analysis

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Separation and quantification of amphetamine enantiomers are commonly used to distinguish between consumption of prescription amphetamine (mostly S-amphetamine) and illicit forms of the drug (racemate). In this study, electromembrane extraction with prototype conductive vials was combined with ultra-high performance supercritical fluid chromatography (UHPSFC-MS/MS) to quantify R-and Samphetamine in urine. Amphetamine was extracted from 100 μL urine, diluted with 25 μL internal standard solution and 175 μL 130 mM formic acid, across a supported liquid membrane (SLM) consisting of 9 μL of a 1:1(w/w) mixture of 2-nitrophenyloctyl ether (NPOE) and bis(2-ethylhexyl)phosphite (DEHPi) into an acceptor phase containing 300 μL 130 mM formic acid. The extraction was facilitated by the application of 30 V for 15 min. Enantiomeric separation was achieved using UHPSFC-MS/MS with a chiral stationary phase. The calibration range was 50-10,000 ng/mL for each enantiomer. The between-assay CV was ≤5%, within-assay CV ≤ 1.5%, and bias within ±2%. Recoveries were 83%-90% (CV ≤ 6%), and internal standard corrected matrix effects were 99-105 (CV ≤ 2%). The matrix effects ranged from 96% to 98% (CV ≤ 8%) when not corrected by the internal standard. The EME method was compared with a chiral routine method that employed liquid-liquid extraction (LLE) for sample preparation. Assay results were in agreement with the routine method, and the mean deviation between methods was 3%, ranging from À21% to 31%. Finally, sample preparation greenness was assessed using the AGREEprep tool, which resulted in a greenness score of 0.54 for conductive vial EME, opposed to 0.47 for semi-automated 96-well LLE.

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“…Sayed et al (2021) developed a simple, sensitive and non‐extractive spectrophotometric method for the determination of fluvoxamine maleate. Skaalvik et al (2021) used conductive vial electromembrane extraction with prototype equipment, which was applied for to extract lipophilic basic drugs from the serum. With this equipment, electromembrane extraction was combined with UHPLC–MS/MS, and a method to determine fluvoxamine and metabolites in serum was developed, optimized and validated.…”

Section: Introductionmentioning

confidence: 99%

“…Sayed et al (2021) developed a simple, sensitive and non-extractive spectrophotometric method for the determination of fluvoxamine maleate. Skaalvik et al (2021) Recent studies reported that fluvoxamine may reduce the excessive inflammatory state mediated by the novel coronavirus by regulating the σ-1 receptor (σ1R), so it plays a very important role in the treatment of the novel coronavirus . The study also found that the drug has an anti-inflammatory and potential antiviral effect; early treatment with 100 mg oral fluvoxamine tablet twice daily for 10 days significantly reduced the risk of hospitalization in COVID-19 patients compared with placebo (Sydney et al, 2021;Wen et al, 2022).…”

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confidence: 99%

Pharmacokinetics and bioequivalence studies of fluvoxamine maleate tablets in healthy Chinese subjects

She

Ming‐qu

et al. 2023

Biomedical Chromatography

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Fluvoxamine is a selective serotonin reuptake inhibitor commonly used for various types of depression. The purpose of this study was to evaluate the pharmacokinetics and bioequivalence of fluvoxamine maleate tablets orally on an empty stomach and after a meal in healthy adult Chinese subjects and to preliminarily evaluate their safety. A single-center, randomized, open-label, two-drug, two-period, crossover, single-dose trial protocol was designed. Sixty healthy Chinese participants were enrolled and randomly classified into fasting (n = 30) and fed groups (n = 30). Each week, subjects took fluvoxamine maleate tablets 50 mg orally once as a test preparation or as a reference preparation on an empty stomach/after meals. To evaluate the bioequivalence of test and reference tables, the concentration of fluvoxamine maleate in the plasma of the subjects at different time points after administration was detected by liquid chromatography-tandem mass spectrometry, and pharmacokinetic parameters including the maximum plasma drug concentration (C max ), the time to reach maximum concentration (T max ), the area under the plasma concentration-time curve from time 0 to the last measurable concentration (AUC 0-t ) and the area under the plasma concentration-time curve from time 0 to infinity (AUC 0-∞ ) were calculated. Our data revealed that the 90% confidence intervals of the geometric mean ratio of the test or reference drugs for the C max , AUC 0-t and AUC 0-∞ fell within the acceptance range for bioequivalence (92.30-102.77%). The absorption, measured by AUC, did not show a significant difference between the two groups. There were no suspected serious adverse reactions or serious adverse events over the entire trial.Our results demonstrated that the test and reference tablets were bioequivalent under fasting and fed conditions.

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Determination of psychoactive drugs in serum using conductive vial electromembrane extraction combined with UHPLC-MS/MS

Cited by 25 publications

References 36 publications

A novel three‐dimensional printed device with conductive elements for electromembrane extraction combined with high‐performance liquid chromatography and ultraviolet detector

A novel three‐dimensional printed device with conductive elements for electromembrane extraction combined with high‐performance liquid chromatography and ultraviolet detector

Determination of amphetamine enantiomers in urine by conductive vial electromembrane extraction and ultra‐high performance supercritical fluid chromatography tandem mass spectrometry

Pharmacokinetics and bioequivalence studies of fluvoxamine maleate tablets in healthy Chinese subjects

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