干旱区生态环境知识资源中心(Arid): Isocyanate derivatization coupled with phospholipid removal microelution-solid phase extraction for the simultaneous quantification of (S)-metoprolol and (S)-alpha-hydroxymetoprolol in human plasma with LC-MS/MS

Arid

DOI	10.1016/j.jpba.2021.114263
	Isocyanate derivatization coupled with phospholipid removal microelution-solid phase extraction for the simultaneous quantification of (S)-metoprolol and (S)-alpha-hydroxymetoprolol in human plasma with LC-MS/MS
	Meloche, Maxime; Jutras, Martin; St-Jean, Isabelle; de Denus, Simon; Leclair, Gregoire
通讯作者	Leclair, G (corresponding author), Univ Montreal, Fac Pharm, CP 6128,Succursale Ctr Ville, Montreal, PQ H3T 1J4, Canada.
来源期刊	JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
ISSN	0731-7085
EISSN	1873-264X
出版年	2021
卷号	204
英文摘要	A sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) assay was developed and validated for the quantification of (S)-metoprolol (MET) and its main metabolite, (S)-alpha-hydroxymetoprolol (OH-MET). Human plasma samples (50 mu L) were spiked with both analytes and their deuterated internal standards (IS) (S)-MET-(d7) and alpha-OH-MET-(d5). Phospholipid removal microelution-solid phase extraction (PRM-SPE) was performed using a 4-step protocol with Oasis PRiME MCX mu Elution 96-well cartridges. The eluates were reconstituted in 100 mu L of acetonitrile with 50 mu gImL (S)-alpha-methylbenzyl isocyanate (MBIC) for chiral derivatization. After 60 min at room temperature, the reaction was quenched using 100 mu L of water 2 % formic acid. Chromatographic separation of the derivatized analytes was performed on a Kinetex phenyl-hexyl core-shell stationary phase with an elution gradient. Mobile phases were composed of a mixture of water and methanol, with ammonium formate and formic acid as buffers. Total runtime was 15 min. Analyte detection was performed by an AB/SCIEX 4000 QTRAP mass spectrometer with multiple reaction monitoring. Chromatograms showed MBIC successfully reacted with racemic MET, alpha-OH-MET, and their respective IS. Detection by positive electrospray ionization did not reveal derivatized by-products. Quantification ranges were validated for (S)-MET and (S)-alpha-OH-MET between 0.5-500 and 1.25-500 ng/mL, respectively, with correlation coefficients (r(2)) >0.9906. The PRM-SPE assay showed low matrix effects (86.9-104.0 %) and reproducible recoveries (69.4-78.7 %) at low, medium, and high quality control (QC) levels. Precision and accuracy were all comprised between 85-115 % for all three QCs, and between 80-120 % for the lower limit of quantification, for intra- and inter-day values (n = 6, 3 consecutive days). Non-derivatized analytes were stable at room temperature, after 3 freeze-thaw cycles, and stored for 30 days at -80 degrees C (n = 4). Reinjection reproducibility of a previously validated batch was achieved after 8 days under auto-sampler conditions, indicating the stability of (S)-MET and (S)-alpha-OH-MET derivatives. Its clinical use was established in a cohort of 50 patients and could be used to further investigate the clinical impact of (S)-MET concentrations. (C) 2021 Elsevier B.V. All rights reserved.
英文关键词	Metoprolol Phospholipid removal microelution-solid phase extraction Isocyanate derivatization LC-MS/MS Chiral assay
类型	Article
语种	英语
收录类别	SCI-E
WOS记录号	WOS:000686903700009
WOS关键词	PERFORMANCE LIQUID-CHROMATOGRAPHY ; MASS-SPECTROMETRY ; HUMAN URINE ; ALPHA-HYDROXYMETOPROLOL ; METOPROLOL ENANTIOMERS ; HEART-FAILURE ; S-METOPROLOL ; METABOLITES ; ENANTIOSELECTIVITY ; MICROEXTRACTION
WOS类目	Chemistry, Analytical ; Pharmacology & Pharmacy
WOS研究方向	Chemistry ; Pharmacology & Pharmacy
资源类型	期刊论文
条目标识符	http://119.78.100.177/qdio/handle/2XILL650/363987
作者单位	[Meloche, Maxime; Jutras, Martin; St-Jean, Isabelle; de Denus, Simon; Leclair, Gregoire] Univ Montreal, Fac Pharm, CP 6128,Succursale Ctr Ville, Montreal, PQ H3T 1J4, Canada; [Meloche, Maxime; de Denus, Simon] Montreal Heart Inst, Montreal, PQ H1T 1C8, Canada; [Meloche, Maxime; de Denus, Simon] Univ Montreal, Saucier Pharmacogen Ctr, Montreal, PQ HIT 1C8, Canada
推荐引用方式 GB/T 7714	Meloche, Maxime,Jutras, Martin,St-Jean, Isabelle,et al. Isocyanate derivatization coupled with phospholipid removal microelution-solid phase extraction for the simultaneous quantification of (S)-metoprolol and (S)-alpha-hydroxymetoprolol in human plasma with LC-MS/MS[J],2021,204.
APA	Meloche, Maxime,Jutras, Martin,St-Jean, Isabelle,de Denus, Simon,&Leclair, Gregoire.(2021).Isocyanate derivatization coupled with phospholipid removal microelution-solid phase extraction for the simultaneous quantification of (S)-metoprolol and (S)-alpha-hydroxymetoprolol in human plasma with LC-MS/MS.JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS,204.
MLA	Meloche, Maxime,et al."Isocyanate derivatization coupled with phospholipid removal microelution-solid phase extraction for the simultaneous quantification of (S)-metoprolol and (S)-alpha-hydroxymetoprolol in human plasma with LC-MS/MS".JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS 204(2021).