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DOI | 10.1016/j.jpba.2020.113521 |
Development and validation of a liquid chromatography coupled to tandem mass spectrometry method for the simultaneous quantification of five analgesics and sedatives, and six of their active metabolites in human plasma: Application to a clinical study on the determination of neurological death in the intensive care unit | |
Jutras, Martin; Williamson, David; Chasse, Michael; Leclair, Gregoire | |
通讯作者 | Leclair, G |
来源期刊 | JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
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ISSN | 0731-7085 |
EISSN | 1873-264X |
出版年 | 2020 |
卷号 | 190 |
英文摘要 | A sensitive and selective high-performance liquid chromatographic method coupled to tandem mass spectrometry was developed and validated for the quantification of morphine, hydromorphone, fentanyl, midazolam and propofol and their metabolites morphine-3-beta-D glucuronide, morphine- 6-beta-D glucuronide, hydromorphone 3-beta-D glucuronide, 1'-hydroxymidazolam-beta-D glucuronide, alpha-hydroxymidazolam and 4-hydroxymidazolam in human plasma using potassium oxalate/sodium fluoride mixture as anticoagulant. Human plasma samples (0.4 mL) to which were added a mixture of eleven deuterated internal standards were subjected to solid phase extraction using a mixed-mode polymeric Oasis PRiME MCX in 96-well format. Propofol was selectively eluted and further derivatized using 2-Fluoro-1-methylpyridinium p-toluenesulfonate, whereas the remaining 10 analytes were eluted separately and further concentrated. The derivatized propofol was analyzed separately in a second injection. The analytes were chromatographically separated on a Kinetex phenyl-hexyl analytical column in gradient elution mode, using a mobile phase consisting of aqueous ammonium formate/formic acid buffer and methanol. The overall run time was 8 min. Detection was performed using an AB/SCIEX 4000 QTRAP instrument with positive electrospray ionization employing scheduled multiple reaction monitoring mode. The lower limits of quantification ranged from 0.02 to 5 ng/mL depending on the analyte. Calibration curves covered a concentration range of 1000x in all cases but 1'-hydroxymidazolam-beta-D-glucuronide where it covered a range of 500 x . The validated method was accurate and precise, the intra-day accuracy and precision of quality control samples (4 concentration levels, n = 6 each) being within 91.5-112 % and 1.3-13.2 % (coefficient of variation), respectively, and inter-day (n = 24; 4 days) accuracy and precision of quality control samples (3 concentration levels) being within 94.8-103.5 % and 3.2-11.2 % (coefficient of variation). Mean absolute extraction recoveries were above 60 % for all compounds, except for hydromorphone 3-beta-D-glucuronide (44 %) and for 1'-hydroxymidazolam-beta-D-glucuronide (33 %). Internal standard corrected matrix effect ranged from -4.8 to 3.8 % in normal plasma and in plasma containing 1 % hemolyzed blood. Analytes were stable (above 90 %) in plasma and blood for 19 hat 22 degrees C, in blood for 90 hat 5 degrees C, in plasma for 60 days at -20 degrees C, for 4 months at -70 degrees C and after three freeze-thaw cycles, and in the injection solvent for at least 3 days in the autosampler. The present method is successfully being applied in a multicenter clinical study for the analysis of plasma samples from patients in intensive care units from a number of Canadian hospitals. (C) 2020 Elsevier B.V. All rights reserved. |
英文关键词 | Method validation Liquid chromatography coupled to tandem mass spectrometry Human plasma Sedatives Analgesics Neurological death |
类型 | Article |
语种 | 英语 |
收录类别 | SCI-E |
WOS记录号 | WOS:000573434900024 |
WOS关键词 | SOLID-PHASE EXTRACTION ; PROPOFOL ; MIDAZOLAM ; MORPHINE ; FENTANYL ; ASSAY ; MORPHINE-6-BETA-GLUCURONIDE ; MORPHINE-3-BETA-GLUCURONIDE ; HYDROMORPHONE ; NORFENTANYL |
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/2XILL650/326542 |
作者单位 | [Jutras, Martin; Williamson, David; Leclair, Gregoire] Univ Montreal, Fac Pharm, Platform Biopharm, Pavillon Jean Coutu,2940 Chemin Polytech, Montreal, PQ H3T 1J4, Canada; [Williamson, David] Hop Sacre Coeur Montreal, Res Ctr, Montreal, PQ H4J 1C5, Canada; [Williamson, David] Hop Sacre Coeur Montreal, Pharm Dept, Montreal, PQ H4J 1C5, Canada; [Chasse, Michael] Univ Montreal, Fac Med, Montreal, PQ H3T 1J4, Canada; [Chasse, Michael] Ctr Hosp Univ Montreal, Res Ctr, Montreal, PQ H2X 0A9, Canada; [Chasse, Michael] Ctr Hosp Univ Montreal, Dept Med Crit Care, Montreal, PQ H2X 0A9, Canada |
推荐引用方式 GB/T 7714 | Jutras, Martin,Williamson, David,Chasse, Michael,et al. Development and validation of a liquid chromatography coupled to tandem mass spectrometry method for the simultaneous quantification of five analgesics and sedatives, and six of their active metabolites in human plasma: Application to a clinical study on the determination of neurological death in the intensive care unit[J],2020,190. |
APA | Jutras, Martin,Williamson, David,Chasse, Michael,&Leclair, Gregoire.(2020).Development and validation of a liquid chromatography coupled to tandem mass spectrometry method for the simultaneous quantification of five analgesics and sedatives, and six of their active metabolites in human plasma: Application to a clinical study on the determination of neurological death in the intensive care unit.JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS,190. |
MLA | Jutras, Martin,et al."Development and validation of a liquid chromatography coupled to tandem mass spectrometry method for the simultaneous quantification of five analgesics and sedatives, and six of their active metabolites in human plasma: Application to a clinical study on the determination of neurological death in the intensive care unit".JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS 190(2020). |
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