Morphine, in biological samples

F. Tagliaro, D. Franchi, R. Dorizzi and M. Marigo, High-performance liquid chromatographic determination of morphine in biological samples an overview of separation methods and detection techniques, J. Chromatogr., 1989, 488, 215-228. 

Complications of drug analysis were successfully resolved by the combination of TLC with MALDI-MS. TLC combined with MALDI-MS was used for analysis of psychotropic drugs (3,4-methylenedioxy methamphetamine, 4-hydroxy-3-methoxy methamphetamine, 3,4-methylenedioxy amphetamine, methamphetamine, p-hydroxy methamphetamine, amphetamine, ketamine, caffeine, chlorpromazine, triazolam, and morphine) in biological samples [42]. This technique was able to analyze 3,4-methylenedioxy methamphetamine (MDMA) and its metabolites in urine samples without sample dilution, and the detection limit of the MDMA spot was 0.05 ng/ spot. Crecelius and coworkers described the use of TLC with MALDI-MS/MS for the structural analysis of small drug molecules [43]. This method was successfully applied to analyze two representatives of nonsteroidal antiinflammatory drugs (tenoxi-cam and piroxicam), and pharmaceutically active compound UK-137,457 and one of its related substances UK-124,912. The feasibility of UTLC-atmospheric pressure (AP)-MALDI-MS was described for the analysis of small molecules (triazole, midazolam, verapamil, and metaprolol) [44]. The authors compared the selectivity and sensitivity between UTLC- and HPTLC-AP-MALDI-MS. It was observed that UTLC plates provided 10-100 times better sensitivity in MALDI analysis than the conventional... 

Morphine in Biological Samples by Gas Chromatography with Electron Capture Detection... 

For the purposes of investigating the disposition of heroin and its metabolites in heroin users, Goldberger et al. developed a GC/MS assay for heroin, 6-AM and morphine in biological fluids, including hair. Hair samples were obtained from subjects who had been enrolled in an outpatient maintenance and detoxification study. 6-AM and morphine were present in all samples heroin was present in 35% of the samples. Codeine was also present in 75% of the samples. The concentrations of 6-AM in hair generally predominated over those of heroin, morphine, and codeine. 

Reverse phase methods were also used to assay dimethylaminoetoposide (2) together with a stereoisomer and their AT-demethylated metabolites in the urine of cancer patients. A related paper discusses an analytical method for etoposide and isomers in plasma. Other work describes the isolation of glucuronides of metronidazole (3) and its hydroxy metabolite (4) by preparative HPLC methods, and the antipyrene metabolite derivatives 5-7 were identified by thermospray LC-MS methods. In the area of the metabolites of narcotics, two papers have described the reverse phase-HPLC analysis of morphine and its 3-and 6-glucuronides in biological samples. In the first case, fluorescence detection was used, in the latter electrospray MS procedures. Codeine and seven glycosidic metabolites have also been analysed by reverse phase-HPLC procedures with UV or electrochemical detection. ... 

The MIPs have also been utilized as the recognition elements in pseudoimmunoassays. " In this approach, MIPs are substituted for antibodies to quantify the amount of analyte in a biological sample, such as blood plasma. Most MIP immunoassays are competitive binding studies in which a radio- or fluorescent-labeled analyte is added to a mixture of the MIP and imlabeled analyte. After equilibrium is reached, some fraction of the labeled species is bound to the polymer surface and thus can be separated from the supernatant. The supernatant is then analyzed via scintillation or fluorescence techniques to determine the concentration of the original unlabeled analyte. Mosbach et al. have demonstrated that MIP-based immunoassays can rival the selectivity of antibody-based assays. Imprinted polymers for the opioid receptor ligands enkephalin and morphine were prepared and showed submicromolar (pM) level selectivity in a radioligand competition assay in aqueous buffers. The analysis... 

Considering the ability of directly analyzing such complex mixtures, crude extracts or even whole biological samples, DADI/MIKE spectrometry and analogous methods are obviously very suitable for screening tests. This has been utilized for the direct analysis not only of the coca leaves of cocaine but also of the constituents in mushrooms (Helvella esculenta ) of morphine, papaverine, coniine, and atropine in plant materials with a detection limit of about 1 to 10 ng of alkaloid , and for the identification of other alkaloids linke ubine, mescaline, hordenine, and uberine in crude cacti extracts . ... 

The discovery of /3-chloromorphide in samples of illicit opiates<241) led an NIH group 198) to investigate their chemical and biological properties. /3-Halomorphides, like their a-counterparts, were found by H nmr to possess an axially positioned halide. Both series are more potent as analgesics than morphine (e.g., /3-chloromorphide has a MHP, sc, ED50 of 0.8mg/kg). They possess all the adverse properties of opiates and have also been shown to be more toxic than morphine. 

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