Simultaneous analysis of Thebaine, 6-MAM and six abused opiates in postmortem fluids and tissues using Zymark® automated solid-phase extraction and gas chromatography–mass spectrometry

Lewis, Russell J.; Johnson, Robert D.; Hattrup, R.A.

doi:10.1016/j.jchromb.2005.05.031

Cited by 45 publications

(29 citation statements)

References 24 publications

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“…OXY concentrations were measured by gas chromatography-MS and represent the total drug (protein or antibodybound as well as free) in each sample. Extraction and quantitation of OXY in brain and serum samples was based on a previously described method (Lewis et al, 2005) using d 6 -OXY as internal standard (Cerilliant Corporation, Round Rock, TX), solid-phase extraction, derivatization with N,O-bis(trimethylsilyl)trifluoroacetamide in 1% trimethylchlorosilane, and analysis on an Agilent 6890 gas chromatograph with methyl siloxane capillary column and 5973 quadrupole mass spectrometer (Agilent Technologies, Santa Clara, CA). Adaptations to the method included omission of NaF, analysis of 0.5-ml samples rather than 3-ml samples, and an initial 1:4 rather than 1:2 dilution of brain into 0.1 M phosphate buffer pH 6.0, and solid-phase extraction of brain homogenate supernatant rather than whole homogenate.…”

Section: Oxy(hs)mentioning

confidence: 99%

An Oxycodone Conjugate Vaccine Elicits Drug-Specific Antibodies that Reduce Oxycodone Distribution to Brain and Hot-Plate Analgesia

Pravetoni

Naour²,

Harmon

et al. 2012

J Pharmacol Exp Ther

123

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Opioid conjugate vaccines have shown promise in attenuating the behavioral effects of heroin or morphine in animals. The goal of this study was to extend this approach to oxycodone (OXY), a commonly abused prescription opioid. Haptens were generated by adding tetraglycine (Gly) 4 or hemisuccinate (HS) linkers at the 6-position of OXY. Immunization of rats with OXY(Gly) 4 conjugated to the carrier proteins bovine serum albumin (BSA) or keyhole limpet hemocyanin (KLH) produced high-titer antibodies to OXY and its metabolite oxymorphone with substantially lower affinities for other structurally related opioid agonists and antagonists. There was no measurable binding of antibody by the (Gly) 4 linker alone or off-target opioids methadone and buprenorphine. OXY(HS) conjugates were less immunogenic despite achieving protein haptenation ratios comparable to OXY(Gly) 4 -BSA. In rats given a single intravenous dose of OXY, immunization with OXY(Gly) 4 -KLH increased OXY protein binding and retention in serum while decreasing its unbound (free) concentration in plasma and distribution to brain. Vaccine efficacy correlated with serum antibody titers, and it was greatest in rats given the lowest OXY dose (0.05 mg/kg) but was significant even after a larger OXY dose (0.5 mg/kg), equivalent to the high end of the therapeutic range in humans. These effects of OXY(Gly) 4 -KLH on drug disposition were comparable to those of nicotine or cocaine vaccines that are in clinical trials as addiction treatments. Immunization with OXY(Gly) 4 -KLH also reduced OXY analgesia in a thermal nociception test. These data support further study of vaccination with the OXY(Gly) 4 -KLH immunogen as a potential treatment option for OXY abuse or addiction.

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Section: Oxy(hs)mentioning

confidence: 99%

An Oxycodone Conjugate Vaccine Elicits Drug-Specific Antibodies that Reduce Oxycodone Distribution to Brain and Hot-Plate Analgesia

Pravetoni

Naour²,

Harmon

et al. 2012

J Pharmacol Exp Ther

123

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“…There are also other methods described in the literature, such as oxidative colorimetric analysis [22], determination of opiates by circular dichroism [23], colorimetric determination [24], TLC analysis of opiate alkaloids and drugs [25,26], ELISA (enzyme-linked immunosorbent assay) analysis of thebaine [27], FTIR spectroscopy of opiates and chemometric analysis [28], differential pulse polarography [29] and even a voltammetric analysis of thebaine [30]. (6) and noscapine (7) T a b l e 2 [31], gas chromatography-ion trap mass spectrometry (GC-MS) analysis [32], liquid chromatographicatmospheric pressure chemical ionization mass spectrometric analysis [33] or HPLC analysis [34,35], GC-MS analysis [36][37][38][39]. Alkaloids are also being analyzed in environmental studies to trace the pollution of the environment [40].…”

Section: Introductionmentioning

confidence: 99%

Development of chromatographic methods for thebaine detection and quantification along with some of related alkaloid derivatives

Spasevska

Bogdanov

Babunovska³

2015

Maced. J. Chem. Chem. Eng.

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A RP-HPLC-UVD method for qualitative analysis and quantification of thebaine was developed utilizing RP-C18 monolithic column, gradient elution with trifluoroacetic acid and formic acid in water and in acetonitrile and detection wavelength of 285 nm. The effects of the relevant chromatographic conditions were investigated and the optimized and validated method was usеd for analysis of three in-house prepared batches of thebaine. Additionally, a complementary GC-MS method was developed for identification of thebaine and potential impurities. In parallel the batches were analyzed by routine methods for preliminary quality assessment based on physical and spectroscopic properties (melting point, specific optical rotation, UV-Vis and IR spectroscopy). There was correlation between the samples purity as determined by the developed HPLC method and the melting point ranges. The HPLC method herein presented is suitable for routine quantitative analysis regardless of the method of thebaine preparation and it is suitable for its corresponding free base or salt form. Additionally, considering the mobile phase compatibility, it can be adapted/transferred easily for HPLC-MS analysis, especially if the identity of the impurities needs to be determined.Keywords: thebaine; HPLC; purity; GC-MS; physical properties; spectroscopic properties; РАЗВОЈ НА ХРОМАТОГРАФСКИ МЕТОДИ ЗА ДЕТЕКЦИЈА И КВАНТИФИКАЦИЈА НА ТЕБАИН ЗАЕДНО СО НЕКОИ СРОДНИ АЛКАЛОИДНИ ДЕРИВАТИMетодатa RP-HPLC-UVD за квалитативна анализа и квантификација на тебаин е развиена со користење на монолитна колона RP-C18. Методата е со градиентна елуција со трифлуорооцетна и мравја киселина во вода и ацетонитрил и со детекција на 285 nm. Беа евалуирани ефектите на релевантните хроматографски услови и оптимизираната и валидирана метода беше применета за анализа на три подготвени серии тебаин. Дополнително беше развиена комплементарна GC-MS метода за идентификација на тебаин и потенцијалните нечистотии. Паралелно со хромато-графските методи, примероците на тебаин беа анализирани со рутински методи за прелиминарно одредување на квалитет, базирани на физички и спектроскопски својства (температура на топење, оптичка ротација, УВ-видлива и инфрацрвена спектроскопија). Постои корелација помеѓу чистотата на примероците одредена со HPLC и соодветните опсези на температурите на топење. Прикажаната HPLC метода е соодветна за рутинска анализа без разлика на методата на подготовка и може да се користи за тебаин како слободна база и за негови соли. Додатно, ако се земе предвид компатибилноста на мобилната фаза, развиената метода лесно може да се адаптира/трансферира за анализи со HPLC-MS, особено ако е потребно да се одреди идентитетот на нечистотиите.Клучни зборови: тебаин; HPLC; GC-MS; физички својства; спектроскопски својства; M. Spasevska, J. Bogdanov, H. Babunovska Maced. J. Chem. Chem. Eng. 34 (2), 231-243 (2015) 232

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“…Compared with conventional organic solvents, ILs possess several attractive properties, for example, a wide electrochemical window, nonvolatility, good conductivity and high viscosity, high chemical and thermal stability (Zhang et al, 2003;Qi et al, 2004). As separation media, ILs have made significant contributions in recent decades in advancing research in HPLC (Laremore et al, 2007;Berthod et al, 2005), GC (Ding et al, 2004) and CE (Lewis et al, 2005;Bao et al, 2008;Qin et al, 2003).…”

Section: Introductionmentioning

confidence: 99%

Simultaneous determination of methylephedrine and pseudoephedrine in human urine by CE with electrochemiluminescence detection and its application to pharmacokeinetics

Liu

Tian

Jia

et al. 2009

Biomedical Chromatography

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A novel method for the determination of ephedra alkaloids (methylephedrine and pseudoephedrine) was developed by electrophoresis capillary (CE) separation and electrochemiluminesence detection (ECL). The use of ionic liquid (1-butyl-3-methylimidazolium tetrafluoroborate, BMIMBF(4)) improved the detection sensitivity markedly. The conditions for CE separation, ECL detection and effect of ionic liquid were investigated in detail. The two ephedra alkaloids with very similar structures were well separated and detected under the optimum conditions. The limits of detection (signal-to-noise ratio = 3) in standard solution were 1.8 x 10(-8) mol/L for methylephedrine (ME) and 9.2 x 10(-9) mol/L for pseudoephedrine (PSE). The limits of quantitation (signal-to-noise ratio = 10) in human urine samples were 2.6 x 10(-7) mol/L for ME and 3.6 x 10(-7 )mol/L for PSE. The recoveries of two alkaloids at three different concentration levels in human urine samples were between 81.7 and 105.0%. The proposed method was successfully applied to the determination of ME and PSE in human urine and the monitoring of pharmacokinetics for PSE. The proposed method has potential in therapeutic drug monitoring and clinical analysis.

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Simultaneous analysis of Thebaine, 6-MAM and six abused opiates in postmortem fluids and tissues using Zymark® automated solid-phase extraction and gas chromatography–mass spectrometry

Cited by 45 publications

References 24 publications

An Oxycodone Conjugate Vaccine Elicits Drug-Specific Antibodies that Reduce Oxycodone Distribution to Brain and Hot-Plate Analgesia

An Oxycodone Conjugate Vaccine Elicits Drug-Specific Antibodies that Reduce Oxycodone Distribution to Brain and Hot-Plate Analgesia

Development of chromatographic methods for thebaine detection and quantification along with some of related alkaloid derivatives

Simultaneous determination of methylephedrine and pseudoephedrine in human urine by CE with electrochemiluminescence detection and its application to pharmacokeinetics

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