A Rapid and Sensitive High-Performance Liquid Chromatography-Electrospray Ionization-Triple Quadrupole Mass Spectrometry Method for the Quantitation of Oxycodone in Human Plasma

Abstract

A sensitive method for the determination of oxycodone concentrations in plasma by high-performance liquid chromatography (HPLC)-electrospray ionization-triple quadrupole mass spectrometry is described. The method is rugged, reliable, selective, and rapid with a run time of 2 min. One milliliter of plasma is made basic and extracted with 2-mL duplicate portions of 2% isoamyl alcohol in n-butyl chloride. The combined extracts are then evaporated to dryness, reconstituted in 100 microL of the mobile phase (15% methanol-85% water containing 0.1% acetic acid), and injected onto the HPLC. The limit of quantitation is 1 ng/mL, and the estimated limit of detection is 33 pg/mL (signal-to-noise = 3). Standard curves are linear over the range of 1 to 100 ng/mL with all correlation coefficient values greater than 0.9989. The method is used to determine the concentration of oxycodone in human plasma following the intravenous infusion of doses ranging from 5 to 15 mg in which the analysis of over 3000 plasma samples is required.

Oxycodone induces overexpression of P‐glycoprotein (ABCB1) and affects paclitaxel's tissue distribution in Sprague Dawley rats

“…Liquid chromatography conditions were optimized through modification of a previously described method. 29 The analytical system consisted of a (1) Finnigan MAT Spectra System coupled to a Finnigan LCQ quadrupole ion trap mass spectrometer, (2) Zorbax SB C-18 (2.1 × 50 mm) (Agilent, Palo Alto, CA), and (3) the mobile phase consisted of acetonitrile:water (0.1% acetic acid) 15:85, while the column temperature was maintained at 60°C, and the flow rate was maintained at 0.2 mL/min. The ions monitored included MH + 316.4 for oxycodone and MH + 300.4 for codeine.…”

Analysis of oxycodol and noroxycodol stereoisomers in biological samples by capillary electrophoresis

“…Methods reported in the literature for the analysis of OCOD and some of its metabolites in various biological matrices feature a variety of techniques, including mass spectrometry (MS) and NMR [8], thin-layer chromatography [8,10], gas chromatography (GC), often coupled to MS detection [7,12,[20][21][22], high-performance liquid chromatography (HPLC) with MS [23], electrochemical [24,25] or UV [15,17] detection, and capillary electrophoresis (CE) with multiwavelength UV [14] and MS detection [14,16].…”

The use of liquid chromatography/mass spectrometry for quantitative analysis of oxycodone, oxymorphone and noroxycodone in Ringer solution, rat plasma and rat brain tissue

“…Some methods also describe measurement of oxymorphone and/or noroxycodone in biological matrices such as plasma 3 or urine, [4][5][6] but the majority of methods are designed for measurement of the parent drug in plasma. [7][8][9][10] The techniques utilize electrochemical detection, 9,10 capillary gas chromatography (GC) 8 and capillary electrophoresis (CE)/ion trap multiple stage mass spectrometry, 4 as well as GC/MS 3,5,6 and liquid chromatography/tandem mass spectrometry (LC/MS/ MS). 7 However, none of these methods supply sufficient analytical sensitivity to allow simultaneous analysis of oxycodone and its metabolites oxymorphone and noroxycodone given the sample volumes provided when working with small animals and the low concentrations and very small sample volumes obtained from microdialysis.…”

“…[7][8][9][10] The techniques utilize electrochemical detection, 9,10 capillary gas chromatography (GC) 8 and capillary electrophoresis (CE)/ion trap multiple stage mass spectrometry, 4 as well as GC/MS 3,5,6 and liquid chromatography/tandem mass spectrometry (LC/MS/ MS). 7 However, none of these methods supply sufficient analytical sensitivity to allow simultaneous analysis of oxycodone and its metabolites oxymorphone and noroxycodone given the sample volumes provided when working with small animals and the low concentrations and very small sample volumes obtained from microdialysis. Compared with the previously described LC/MS/MS method, 7 the use of direct injection or work-up procedures without the need to silanize glassware results in a faster and less hazardous sample preparation.…”

“…7 However, none of these methods supply sufficient analytical sensitivity to allow simultaneous analysis of oxycodone and its metabolites oxymorphone and noroxycodone given the sample volumes provided when working with small animals and the low concentrations and very small sample volumes obtained from microdialysis. Compared with the previously described LC/MS/MS method, 7 the use of direct injection or work-up procedures without the need to silanize glassware results in a faster and less hazardous sample preparation. The use of MS provides high sensitivity and high selectivity, and the use of an LC system reduces the effort needed for work-up of the samples compared with GC.…”