Citation: XU Duo-Qi, ZHANG Lei-Ping, WANG Ji-Fen, HUANG Jian, GUO Zhen, LIN Kuan. Determination of Zaleplon and Its Metabolites in Human Blood by QuEChERS-Ultra Performance Liquid Chromatography-Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, ;2016, 44(7): 1059-1064. doi: 10.11895/j.issn.0253-3820.160033 shu

Determination of Zaleplon and Its Metabolites in Human Blood by QuEChERS-Ultra Performance Liquid Chromatography-Mass Spectrometry

1.
College of Criminal Science and Technology, People's Public Security University of China, Beijing 100038, China;
2.
Institute of Forensic Science, Ministry of Public Security, Beijing 100038, China

Received Date: 13 January 2016
Revised Date: 14 April 2016

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A fast testing method was established for the determination of zaleplon and its two metabolites, 5-oxozaleplon and desethylzaleplon, in blood by ultra performance liquid chromatography tandem electrospray ionization triple quadrapole-mass spectrometry (UPLC-TQ/MS). The optimized QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method was used for sample preparation. The blood samples were extracted with 0.1% acetic acid and dehydrated by adding anhydrous magnesium sulfate. The targets were separated on a Waters BEH C₁₈ column by gradient elution with 0.1% formic acid-0.1% formic acid/acetonitrile as mobile phase, ionized with positive electrospray (ESI⁺), and detected under multiple reaction monitoring (MRM) mode. As a result, zaleplon and its two metabolites displayed excellent linearity in the concentration of 0.5-100 ng/mL (R²>0.997). The average recoveries ranged from 92.0% to 100.1%. The RSD were in the range of 1.9%-5.3%. Besides, the limit of detection(LOD)of this method for target drugs was 0.05 ng/mL (S/N=3), while limits of quantification (LOQ) were in the range of 0.1-0.5 ng/mL (S/N=10). This method can meet the demand of rapidity and accuracy in the analysis of actual cases.
- Zaleplon,
- 5-Oxozaleplon,
- Desethylzaleplon,
- QuEChERS,
- Ultra performance liquid chromatography-mass spectrometry
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1.
沈阳化工大学材料科学与工程学院沈阳 110142