scholarly journals Quantitation of fentanyl analogs in dried blood spots by flow-through desorption coupled to online solid phase extraction tandem mass spectrometry

2017 ◽  
Vol 9 (25) ◽  
pp. 3876-3883 ◽  
Author(s):  
Rebecca L. Shaner ◽  
Nicholas D. Schulze ◽  
Craig Seymour ◽  
Elizabeth I. Hamelin ◽  
Jerry D. Thomas ◽  
...  
Keyword(s):  
Solid Phase Extraction ◽  
Solid Phase ◽  
Dried Blood Spots ◽  
Spectrometric Analysis ◽  
Tandem Mass ◽  
Phase Extraction ◽  
Online Solid Phase Extraction ◽  
Fentanyl Analogs ◽  
Flow Through ◽  
Tandem Mass Spectrometric

An automated dried blood spot (DBS) elution coupled with solid phase extraction and tandem mass spectrometric analysis for multiple fentanyl analogs was developed and assessed.

scholarly journals Plasma Free Metanephrine Measurement Using Automated Online Solid-Phase Extraction HPLC–Tandem Mass Spectrometry

2007 ◽  
Vol 53 (9) ◽  
pp. 1684-1693 ◽  
Author(s):  
Wilhelmina HA de Jong ◽  
Kendon S Graham ◽  
Jan C van der Molen ◽  
Thera P Links ◽  
Michael R Morris ◽  
...  
Keyword(s):  
Solid Phase Extraction ◽  
Solid Phase ◽  
Mass Spectrometric ◽  
Mass Spectrometric Detection ◽  
Tandem Mass ◽  
Phase Extraction ◽  
Analytical Sensitivity ◽  
Automated Method ◽  
Online Solid Phase Extraction ◽  
Tandem Mass Spectrometric

Abstract Background: Quantification of plasma free metanephrine (MN) and normetanephrine (NMN) is considered to be the most accurate test for the clinical chemical diagnosis of pheochromocytoma and follow-up of pheochromocytoma patients. Current methods involve laborious, time-consuming, offline sample preparation, coupled with relatively nonspecific detection. Our aim was to develop a rapid, sensitive, and highly selective automated method for plasma free MNs in the nanomole per liter range. Methods: We used online solid-phase extraction coupled with HPLC-tandem mass spectrometric detection (XLC-MS/MS). Fifty microliters plasma equivalent was prepurified by automated online solid-phase extraction, using weak cation exchange cartridges. Chromatographic separation of the analytes and deuterated analogs was achieved by hydrophilic interaction chromatography. Mass spectrometric detection was performed in the multiple reaction monitoring mode using a quadrupole tandem mass spectrometer in positive electrospray ionization mode. Results: Total run-time including sample cleanup was 8 min. Intra- and interassay analytical variation (CV) varied from 2.0% to 4.7% and 1.6% to 13.5%, respectively, whereas biological intra- and interday variation ranged from 9.4% to 45.0% and 8.4% to 23.2%. Linearity in the 0 to 20 nmol/L calibration range was excellent (R2 > 0.99). For all compounds, recoveries ranged from 74.5% to 99.6%, and detection limits were <0.10 nmol/L. Reference intervals for 120 healthy adults were 0.07 to 0.33 nmol/L (MN), 0.23 to 1.07 nmol/L (NMN), and <0.17 nmol/L (3-methoxytyramine). Conclusions: This automated high-throughput XLC-MS/MS method for the measurement of plasma free MNs is precise and linear, with short analysis time and low variable costs. The method is attractive for routine diagnosis of pheochromocytoma because of its high analytical sensitivity, the analytical power of MS/MS, and the high diagnostic accuracy of free MNs.

scholarly journals Validation of a Solid-Phase Extraction and Ultra-Performance Liquid Chromatographic Tandem Mass Spectrometric Method for the Detection of 16 Glucocorticoids in Pig Tissues

2009 ◽  
Vol 92 (2) ◽  
pp. 604-611 ◽  
Author(s):  
Bing Shao ◽  
Xiaoliang Cui ◽  
Yi Yang ◽  
Jing Zhang ◽  
Yongnin Wu
Keyword(s):  
Solid Phase Extraction ◽  
Solid Phase ◽  
Monitoring Program ◽  
Ion Source ◽  
Tandem Mass ◽  
Phase Extraction ◽  
Mass Spectrometric Method ◽  
Relative Standard ◽  
Liver And Kidney ◽  
Tandem Mass Spectrometric

Abstract A sensitive analytical method has been developed and validated for simultaneous determination of 16 glucocorticoid (fluorometholone, flumethasone, triamcinolone, aldosterone, clobetasol propionate, methylprednisolone, fluocinolone acetonide, hydrocortisone, prednisone, dexamethasone, beclomethasone, prednisolone, budesonide, triamcinolone acetonide, fludrocortisone acetate, and cortisone) residues in pig tissues (muscle, liver, and kidney). These biosamples were hydrolyzed with -glucuronidase/arylsulfatase enzyme and passed through a Supelclean ENVI-Carb graphitized carbon black solid-phase extraction cartridge, followed by further purification using aminopropyl cartridges. Analytes were separated on an ultra-performance liquid chromatography BEH C18 column followed by tandem mass spectrometry (MS) with an electrospray ion source. The MS data acquisition was performed in the negative multireaction monitoring mode by a time-scheduled multireaction monitoring program. The assay for the 16 glucocorticoids were linear over the range of 1250 g/L for pork, liver, and kidney, with correlation coefficient >0.99. Estimated detection limits for the target analytes ranged from 0.03 to 0.30 g/kg, and limits of quantitation ranged from 0.10 to 1.00 g/kg. Recoveries of the glucocorticoids (spiked at levels of 0.4 and 2.0 g/kg) ranged from 81.0 to 112.3, with relative standard deviations between 2.6 and 16.6.

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