title: Development of an SPE method for the determination of zaleplon and zopiclone in hemolyzed blood using fast GC with negative-ion chemical ionization MS.
abstract: 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 Oasis MCX and HLB columns, and sufficient extraction efficiency was achieved at pH 9.0. For further study a hydrophilic-lipophilic sorbent Oasis 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.
authors.affiliation: Center of Nanotechnology and Material Science, Department of Analytical and Environmental Chemistry, Faculty of Chemistry, Vilnius University, Vilnius, Lithuania; State Forensic Medicine Service Under the Ministry of Justice of the Republic of Lithuania, Vilnius, Lithuania.
authors.forename: Nerijus
authors.initials: N
authors.lastname: Karlonas
authors.forename: Arunas
authors.initials: A
authors.lastname: Ramanavicius
authors.forename: Almira
authors.initials: A
authors.lastname: Ramanaviciene
mesh_terms: D000081:Acetamides / Q000097:blood* / Q000302:isolation & purification*; D053961:Azabicyclo Compounds / Q000097:blood* / Q000302:isolation & purification*; D008401:Gas Chromatography-Mass Spectrometry; D006801:Humans; D006993:Hypnotics and Sedatives / Q000097:blood* / Q000302:isolation & purification*; D010879:Piperazines / Q000097:blood* / Q000302:isolation & purification*; D011743:Pyrimidines / Q000097:blood* / Q000302:isolation & purification*; D052616:Solid Phase Extraction / Q000379:methods*
chemical_list: D000081:Acetamides; D053961:Azabicyclo Compounds; D006993:Hypnotics and Sedatives; D010879:Piperazines; D011743:Pyrimidines; C515050:zopiclone; C085665:zaleplon
keywords: Hemolyzed blood; Mixed-mode SPE; Polymeric sorbents; Zaleplon; Zopiclone