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Extraction of ketamine from urine using a miniature silica monolithic cartridge followed by quantification with liquid chromatography tandem mass spectrometry (LC‐MS/MS)
Author(s) -
Nema Tarang,
Chan Eric C. Y.,
Ho Paul C.
Publication year - 2011
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.201000922
Subject(s) - chromatography , solid phase extraction , chemistry , detection limit , monolith , mass spectrometry , cartridge , extraction (chemistry) , ion suppression in liquid chromatography–mass spectrometry , electrospray , electrospray ionization , monolithic hplc column , tandem mass spectrometry , high performance liquid chromatography , liquid chromatography–mass spectrometry , sample preparation , analytical chemistry (journal) , analyte , materials science , biochemistry , metallurgy , catalysis
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.