Extraction of ketamine from urine using a miniature silica monolithic cartridge followed by quantification with liquid chromatography tandem mass spectrometry (LC‐MS/MS)

Abstract

The high surface area monolith with reactive hydroxyl group on its surface enables it to function as a miniature solid-phase extraction (SPE) cartridge in size of 1 cm in diameter and 0.5 cm in length. The prepared silica monolith was characterized by Brunauer-Emmett-Teller method, scanning electron microscopy, X-ray diffraction and Fourier transform infrared (FTIR) spectroscopy. Ketamine was selected as model analyte to validate the extraction efficiency of the prepared cartridge. The extracted ketamine from urine sample was quantitated by liquid chromatography tandem mass spectrometry (LC-MS/MS) using positive electrospray ionization. The limit of detection and quantification for ketamine was found to be 0.5 and 1.6 ng/mL, respectively. The analysis exhibited linearity in the range of 10-500 ng/mL with coefficient of correlation >0.99. The recovery was found to be in the range of 89-107% with relative standard deviation (RSD) less than 10%. The prepared cartridge was found robust in extracting ketamine efficiently and repeatedly without any significant deterioration in its performance. Moreover, the batch-to-batch variations in the performance of the prepared cartridges in terms of % ion suppression of the extracts and recoveries of samples were small, suggesting the consistency in the properties of the monolith.

Ampholine-functionalized hybrid organic–inorganic silica material as sorbent for solid-phase extraction of acidic and basic compounds

“…On the other hand, although silica-based materials offer high mechanical strength, high permeability, and good organic solvent tolerance, their preparation is time-consuming and difficult to control, leading to poor reproducibility [17]. In addition, monolithic materials can be prepared in capillaries, syringes [18][19][20], and even pipette tips [21,22].…”

The pharmacokinetics of ketamine following intramuscular injection to F344 rats

“…Historically, gas chromatography–mass spectrometry (GC–MS) has been a highly useful approach and offers the ability for separation of stereoisomers . Liquid chromatography–mass spectrometry (LC–MS) has also been a favored approach due to its sensitivity and reduced need for complex sample extraction approaches . As both ketamine and norketamine are pharmacologically active, sensitive and selective methodologies are necessary to accurately quantitate both compounds.…”

“…[21][22][23][24][25] Liquid chromatography-mass spectrometry (LC-MS) has also been a favored approach due to its sensitivity and reduced need for complex sample extraction approaches. [26][27][28][29][30][31][32] As both ketamine and norketamine are pharmacologically active, sensitive and selective methodologies are necessary to accurately quantitate both compounds.…”

Construction of a portable sample preparation device with a magnetic poly(methacrylic acid-co-ethylene dimethacrylate) monolith as the extraction medium and its application in the enrichment of UV filters in water samples

“…To address the problem, monoliths were adopted as alternatives to coated fibers owing to their bulk entity, high surface area, high extraction capacity as well as high permeability . Various monolithic materials, polymers , inorganic, or hybrid matrices , were reported for this purpose. Among others, poly(methacrylic acid‐co‐ethylene dimethacrylate) (MAA‐EDMA) was one of the most widely used monolithic materials, for its excellent extraction ability toward basic and hydrophobic analytes and good biocompatibility .…”