scholarly journals A Sensitive and Selective Method for Determination of Aesculin in Cortex Fraxini by Liquid Chromatography Quadrupole Time-of-Flight Tandem Mass Spectrometry and Application in Pharmacokinetic Study

2013 ◽  
Vol 2013 ◽  
pp. 1-6 ◽  
Author(s):  
Yi Li ◽  
Hui Guo ◽  
Yinying Wu ◽  
Qianqian Geng ◽  
Danfeng Dong ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Pharmacokinetic Study ◽  
High Performance ◽  
Time Of Flight ◽  
Internal Standard ◽  
High Sensitivity ◽  
Rat Plasma ◽  
Linear Range ◽  
Tandem Mass ◽  
Tandem Mass Spectrometric

A rapid and sensitive method for determining aesculin of Cortex fraxini in rat was developed using high-performance liquid chromatography (HPLC) quadrupole time-of-flight (QTOF) tandem mass (MS/MS). Rat plasma was pretreated by fourfold methanol to remove plasma proteins. Chromatographic separation was performed on a reverse phase column. A tandem mass spectrometric detection with an electrospray ionization (ESI) interface was achieved using collision-induced dissociation (CID) under positive ionization mode. The MS/MS patterns monitored werem/z341.2716 →m/z179.1043 for aesculin andm/z248.3025 →m/z120.9130 for tinidazole (internal standard). The linear range was calculated to be 10.0–1500.0 ng/mL with a detection limit of 2.0 ng/mL. The inter- and intraday accuracy and precision were within ±7.0%. Pharmacokinetic study showed that aesculin was confirmed to be a one-compartment open model. The method is believed to have good linear range, high sensitivity and recoveries, and superior analytical efficiency. It will probably be an alternative for pharmacokinetic study of aesculin.

scholarly journals Quantification of Warfarin in Dried Rat Plasma Spots by High-Performance Liquid Chromatography with Tandem Mass Spectrometry

2016 ◽  
Vol 2016 ◽  
pp. 1-6 ◽  
Author(s):  
Alexander Chernonosov
Keyword(s):  
Mass Spectrometry ◽  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
High Performance ◽  
Internal Standard ◽  
Rat Plasma ◽  
Negative Ion ◽  
Tandem Mass ◽  
Water Mixture

This paper presents the development and validation of a novel method for quantification of the oral anticoagulant drug warfarin in dried plasma spots (DPS) by high-performance liquid chromatography with tandem mass spectrometry (HPLC-MS/MS). Blood plasma was chosen as a biological fluid to preclude the influence of the hematocrit on the results of the analysis. A 30 μL sample of rat plasma was placed onto Whatman 903 Protein Saver Card and was allowed to dry. A single DPS is sufficient for preparing eight 3.2 mm discs, each containing approximately 1.5–1.6 μL of plasma. Warfarin extraction from one 3.2 mm disc was carried out by adding 200 μL of the acetonitrile : water mixture (1 : 1, v/v) containing 10 mM NH4COOH (pH 4.0), with incubation on a shaker at 1000 rpm for 1 h at 25°C. After chromatographic separation, warfarin and coumachlor (an internal standard) were measured using negative-ion multiple-reaction monitoring with ion transitions m/z 307 → 161 for warfarin and m/z 341 → 161 for the internal standard. The working range of this method is 10–10,000 ng/mL. Within this range, intra- and interday variability of precision and accuracy was <13% and recovery was 82–99%. The results indicate that the new method requires only small plasma samples and may be useful for pharmacokinetic research on warfarin.

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