A method based on gas chromatography-mass spectrometry (GC-MS) is described for the determination of opioids (6-monoacetylmorphine, morphine, methadone and tramadol) and cocaine and its major metabolite in human bone. After the addition of nalorphine as internal standard, pulverized samples were incubated in acetonitrile for 1 h under ultrasounds. After adjusting the pH of the samples to 6, they were subjected to solid phase extraction and the analytes were eluted using 2 ml of dichloromethane/isopropanol/ammonia (78:20:2). Chromatography was performed on a fused silica capillary column and analytes were determined in the selected-ion-monitoring (SIM) mode. The assay was validated in the range 0.3-1 ng/mg (depending on the drug) to 150 ng/mg, the mean absolute recoveries ranging from 66% to 110%, the matrix effect from 62% to 121% and process efficiency from 61% to 89% depending on the analyte. The intra- and inter-assay accuracy values were always better than 20%. The validated method was then successfully applied to real bone samples from forensic cases in which toxicological analysis for these drugs in blood was positive. Drugs were detected in bone in 12 of the 15 blood positive results. The approximate concentration range was 3-5 ng/g for 6-monoacetylmorphine, 3-7 ng/g for morphine, 14-28 ng/g for methadone and 6 ng/g and 11 ng/g for tramadol and benzoylecgonine.

01 Feb 2018·Analytical BiochemistryQ4 · BIOLOGY

Method validation in quantitative analysis of phase I and phase II metabolites of mitragynine in human urine using liquid chromatography-tandem mass spectrometry

Q4 · BIOLOGY

Article

Author: Keng Yoon Yeong ; Mei Jin Lee ; Sharif Mahsufi Mansor ; Soo Choon Tan ; Surash Ramanathan

A method using solid phase extraction and liquid chromatography-tandem mass spectrometry to quantitatively detect mitragynine, 16-carboxy mitragynine, and 9-O-demethyl mitragynine in human urine samples was developed and validated. The relevant metabolites were identified using multiple reaction monitoring in positive ionization mode using nalorphine as an internal standard. The method was validated for accuracy, precision, recovery, linearity, and lower limit of quantitation. The intra- and inter-day accuracy and precision were found in the range of 83.6-117.5% with coefficient of variation less than 13%. The percentage of recovery for mitragynine, 16-carboxy mitragynine, and 9-O-demethyl mitragynine was within the range of 80.1-118.9%. The lower limit of quantification was 1 ng/mL for mitragynine, 2 ng/mL for 16-carboxy mitragynine, and 50 ng/mL for 9-O-demethyl mitragynine. The developed method was reproducible, high precision and accuracy with good linearity and recovery for mitragynine, 16-carboxy mitragynine, and 9-O-demethyl mitragynine in human urine.

01 Feb 2017·Journal of Pharmaceutical and Biomedical AnalysisQ3 · MEDICINE

Physico-chemical profiling of semisynthetic opioids

Q3 · MEDICINE

Article

Author: Mazák, Károly ; Hosztafi, Sándor ; Noszál, Béla ; Kraszni, Márta

Species-specific acid-base and partition equilibrium constants were experimentally determined for the therapeutically important semisynthetic opioid receptor agonist hydromorphone, dihydromorphine, and mixed agonist-antagonist nalorphine and nalbuphine. The acid-base microequilibria were characterized by combining pH-potentiometry and deductive methods using synthesized auxiliary compounds. Independent of the pH, there are approximately 4.8 times as many zwitterionic microspecies than non-charged ones in nalbuphine solutions, while for nalorphine it is the non-charged form that predominates by the same ratio. The non-charged microspecies is the dominant one also in the case of hydromorphone, although its concentration exceeds only 1.3 times that of its zwitterionic protonation isomer. The pH-independent partition coefficients of the individual microspecies were determined by a combination of experimentally measured, pH-dependent, conditional distribution constants and a custom-tailored evaluation method, using highly similar auxiliary compounds. The pH-independent contribution of the zwitterionic microspecies to the distribution constant is 1380, 1070, 3160 and 72,440 times smaller than that of the inherently more lipophilic non-charged one for hydromorphone, dihydromorphine, nalbuphine and nalorphine, respectively.

100 Deals associated with Nalorphine Hydrobromide

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KEGG	Wiki	ATC	Drug Bank
-	Nalorphine Hydrobromide	V03AB02	DB11490

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