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Development of an SPE method for the determination of zaleplon and zopiclone in hemolyzed blood using fast GC with negative‐ion chemical ionization MS
Author(s) -
Karlonas Nerijus,
Ramanavicius Arunas,
Ramanaviciene Almira
Publication year - 2014
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.201300784
Subject(s) - zopiclone , chemistry , sorbent , chromatography , extraction (chemistry) , analyte , gas chromatography , analytical chemistry (journal) , hypnotic , organic chemistry , psychology , adsorption , psychiatry
An SPE procedure for the determination of zaleplon and zopiclone in low‐volume human hemolyzed blood using fast GC with negative‐ion chemical ionization MS has been developed and validated. Both analytes were well retained on O asis MCX and HLB columns, and sufficient extraction efficiency was achieved at pH 9.0. For further study a hydrophilic‐lipophilic sorbent O asis HLB was selected due to the polarity of sorbent surface and its large surface area in order to achieve efficient extraction of both analytes in a single step. Special attention has been paid to choosing washing and eluting solvents, resulting in a particularly/extremely clean and moisture‐free extract. The mean extraction efficiency was higher than 90.1% for zaleplon and 82.9% for zopiclone. The precision for zaleplon and zopiclone was between 3.04–10.58% and 4.08–9.52%, respectively. Whereas the accuracy was in the range from –5.73 to 6.00%, and from –7.00 to 6.32% for zaleplon and zopiclone, respectively. The results show that the developed method is accurate, selective, precise, and very fast with excellent recovery and low LOD and LOQ .