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- Title
在线固相萃取-液质联用法同时检测血液样品中 12种芬太尼类药物.
- Authors
孙立敏; 王松才; 朱焕慧; 林贤文; 管 旭; 谭 莉
- Abstract
Objective To establish a method for simultaneous determination of 12 fentanyl-kind drugs in blood through integral SPE-LC-MS/MS with purpose to provide reference for identification of relevant cases. Methods The blood samples (harboring the 12 fentanyl-kind drugs) were treated with acetonitrile for proteins to precipitate, successively centrifugated to collect the supernatant that was subjected to dilution and filtration. The filtrate was directly undergone into integral SPE-LCMS/MS processing so that Agilent PLRP-S (15-20µm, 2.1mm×12.5mm) column had played its role to enrich and purify the injected filtrate and Agilent Poroshell 120 EC-C18 (3.0mm×150mm, 2.7µm) column to perform its chromatographic separation under the gradient elution of mobile phases of A (5mmol/L ammonium acetate plus 0.1% formic acid) and B (acetonitrile). The analytes were detected in multiple reaction monitoring (MRM) mode through the electrospray positive ionization (ESI+). Results Under the optimization of chromatographic condition, mass spectral setting, sampling flow, mobile phase, valve swithching programs and organic solvent ratio, the 12 fentanyl-kind drugs showed good linear relationship within the tested concentration ranges, revealing their coefficients of determination as R2 >0.9990. The method was present of detection limits and quantification limits being 0.2-0.4ng/mL and 0.7-1.4ng/mL, demonstrating the recoveries at three levels being fallen into 83.1%-131.1%, intra-and inter-day RSDs being the respective 1.0%-25.6% and 2.1%-30.5% (n=6). Conclusions The method established here is simple and efficient, demonstrating its excellence of low quantity of required sample, high sensitivity and low detection limit, suitable for simultaneous determination of 12 fentanyl-kind drugs in blood.
- Subjects
GRADIENT elution (Chromatography); AMMONIUM acetate; FORMIC acid; DETECTION limit; FENTANYL; ORGANIC solvents
- Publication
Forensic Science & Technology, 2022, Vol 47, Issue 2, p121
- ISSN
1008-3650
- Publication type
Article
- DOI
10.16467/j.1008-3650.2021.0167