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[Simultaneous determination of 10 unapproved sedative drugs in feeds by ultra-performance liquid chromatography-quadrupole-time-of-flight mass spectrometry].
- Source :
-
Se pu = Chinese journal of chromatography [Se Pu] 2012 May; Vol. 30 (5), pp. 457-62. - Publication Year :
- 2012
-
Abstract
- A new analytical method using ultra-performance liquid chromatography-quadrupole-time-of-flight mass spectrometry (UPLC-Q-TOF-MS) was developed for screening and confirmation of 10 unapproved sedative drugs in feeds. The samples were extracted using the solution of methanol-0.1 mol/L HCl (9:1, v/v), and the extracts were centrifuged and then directly purified through MCX cartridges. The identification and detection were achieved in positive electrospray ionization (ESI) mode using Q-TOF-MS. The potential of UPLC-Q-TOF MS for confirmatory analysis was shown by determining the accurate mass of all the compounds and fragment ions upon collision-induced-dissociation (CID) at different energies. The extra mass measurement errors for all the sedative drugs were found to be within 5 ppm. The calibration graphs were linear in the concentration range of 5-100 microg/L with the correlation coefficients more than 0.99 for the 10 drugs. The limits of quantification (LOQ, S/N = 10) were 8 microg/kg for nitrazepam, zolpidem and thioridazine; 10 microg/kg for thriazolam, estazolam, diazepam, promethazine, chlorpromazine and midazolam; 20 microg/kg for clozapine. The recoveries for all the compounds in feeds were 60.6%-108.5% with the relative standard deviations less than 10% at the spiked levels of LOQ, 2LOQ and 4LOQ.
Details
- Language :
- Chinese
- ISSN :
- 1000-8713
- Volume :
- 30
- Issue :
- 5
- Database :
- MEDLINE
- Journal :
- Se pu = Chinese journal of chromatography
- Publication Type :
- Academic Journal
- Accession number :
- 22934407
- Full Text :
- https://doi.org/10.3724/sp.j.1123.2011.12032