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Chromatographic Retention Times (chromatographic + retention_time)
Selected AbstractsCharacterization of metabolites of tanshinone IIA in rats by liquid chromatography/tandem mass spectrometryJOURNAL OF MASS SPECTROMETRY (INCORP BIOLOGICAL MASS SPECTROMETRY), Issue 5 2006Peng Li Abstract The metabolism of tanshinone IIA was studied in rats after a single-dose intravenous administration. In the present study, 12 metabolites of tanshinone IIA were identified in rat bile, urine and feces with two LC gradients using LC-MS/MS. Seven phase I metabolites and five phase II metabolites of tanshinone IIA were characterized and their molecular structures proposed on the basis of the characteristics of their precursor ions, product ions and chromatographic retention time. The seven phase I metabolites were formed, through two main metabolic routes, which were hydroxylation and dehydrogenation metabolism. M1, M4, M5 and M6 were supposedly tanshinone IIB, hydroxytanshinone IIA, przewaquinone A and dehydrotanshinone IIA, respectively, by comparing their HPLC retention times and mass spectral patterns with those of the standard compounds. The five phase II metabolites identified in this research were all glucuronide conjugates, all of which showed a neutral loss of 176 Da. M9 and M12 were more abundant than other identified metabolites in the bile, which was the main excretion path of tanshinone IIA and the metabolites. M12 was the main metabolite of tanshinone IIA. M9 and M12 were proposed to be the glucuronide conjugates of two different semiquinones and these semiquinones were the hydrogenation products of dehydrotanshinone IIA and tanshinone IIA, respectively. This hydrogenized reaction may be catalyzed by the NAD(P)H: quinone acceptor oxidoreductase (NQO). The biotransformation pathways of tanshinone IIA were proposed on the basis of this research. Copyright © 2006 John Wiley & Sons, Ltd. [source] Screening strategy for the rapid detection of in vitro generated glutathione conjugates using high-performance liquid chromatography and low-resolution mass spectrometry in combination with LightSight® software for data processingRAPID COMMUNICATIONS IN MASS SPECTROMETRY, Issue 22 2009César Ramírez-Molina The knowledge of drug metabolism in the early phases of the drug discovery process is vital for minimising compound failure at later stages. As chemically reactive metabolites may cause adverse drug reactions, it is generally accepted that avoiding formation of reactive metabolites increases the chances of success of a molecule. In order to generate this important information, a screening strategy for the rapid detection of invitro generated reactive metabolites trapped by glutathione has been developed. The bioassay incorporated the use of native glutathione and its close analogue the glutathione ethyl ester. The generic conditions for detecting glutathione conjugates that undergo constant neutral loss of 129 Da were optimised using a glutathione-based test mix of four compounds. The final liquid chromatography/tandem mass spectrometry constant neutral loss method used low-resolution settings and a scanning window of 200 amu. Data mining was rapidly and efficiently performed using LightSight® software. Unambiguous identification of the glutathione conjugates was significantly facilitated by the analytical characteristics of the conjugate pairs formed with glutathione and glutathione ethyl ester, i.e. by chromatographic retention time and mass differences. The reliability and robustness of the screening strategy was tested using a number of compounds known to form reactive metabolites. Overall, the developed screening strategy provided comprehensive and reliable identification of glutathione conjugates and is well suited for rapid routine detection of trapped reactive metabolites. This new approach allowed the identification of a previously unreported diclofenac glutathione conjugate. Copyright © 2009 John Wiley & Sons, Ltd. [source] Sampling in the Great Lakes for pharmaceuticals, personal care products, and endocrine-disrupting substances using the passive polar organic chemical integrative samplerENVIRONMENTAL TOXICOLOGY & CHEMISTRY, Issue 4 2010Hongxia Li Abstract The passive polar organic chemical integrative sampler in the pharmaceutical configuration (i.e., pharmaceutical-POCIS) was calibrated for sampling at water temperatures of 5, 15 and 25°C to determine the influence of temperature on chemical-specific sampling rates (RS), thus providing more robust estimates of the time-weighted average concentrations of pharmaceuticals and personal care products (PPCPs) and endocrine-disrupting substances (EDS) in surface water. The effect of water temperature and flow on the RS of these analytes was evaluated in the laboratory with a static system. The loss of the test compounds from water by uptake into POCIS was linear over an 8-d period, and these experimental data yielded RS values in the range of 0.07 to 2.46 L/d across the temperature range for the 30 compounds tested. Water temperature and flow influenced POCIS uptake rates, but these effects were relatively small, which is consistent with the theory for uptake into POCIS samplers. Therefore, under a narrow range of water temperatures and flows, it may not be necessary to adjust the RS for POCIS. Except for acidic drugs and sulfonamide antibiotics, RS values were positively correlated with octanol,water partition coefficients (log KOW) of the test compounds. A linear relationship was also observed between RS and chromatographic retention times on a C18 reversed-phase column. These observations may provide a rapid method for estimating the RS of additional chemicals in the POCIS. The application of the RS to POCIS deployed for one month in Lake Ontario, Canada, during the summers of 2006 and 2008 yielded estimates of PPCP and EDS concentrations that are consistent with conventional concentration measurements of these compounds in Lake Ontario surface water. Environ. Toxicol. Chem. 2010;29:751,762. © 2009 SETAC [source] Prediction of gas chromatographic retention times of capillary columns of different inside diametersJOURNAL OF SEPARATION SCIENCE, JSS, Issue 18 2003Kornkanok Aryusuk Abstract The retention times (t R) of n -alkanes (C16,C22) eluted from capillary columns of different diameters are accurately predicted by using the equation proposed by Krisnangkura et al. (J. Chromatogr. Sci.1997, 35, 329,332). The numerical values of four thermodynamically related constants (a, b, c, and d) of the BP-1 (100% dimethylpolysiloxane) capillary column (0.32 mm ID×25 m, film thickness, 0.25 ,m) are ,6.169, ,0.512, 226.98, and 410.30, respectively. For columns of the same stationary phase but of different inside diameters and film thickness, accurate tR values can be predicted by using the same numerical values of the last three constants but the first constant (a) is changed by the difference in the natural logarithm of the column phase ratios (,). All the derived numerical values of each column were tested with FAMEs and with n -alkanes in temperature-programmed GC (TPGC). All the predicted tR values agree well with the experimental values. About 77% of the TPGC data have errors lower than 0.5% and the largest value is ,1.04%. [source] Detection of norbolethone, an anabolic steroid never marketed, in athletes' urineRAPID COMMUNICATIONS IN MASS SPECTROMETRY, Issue 13 2002Don H. Catlin Norbolethone (13-ethyl-17-hydroxy-18,19-dinor-17,-pregn-4-en-3-one) is a 19-nor anabolic steroid first synthesized in 1966. During the 1960s it was administered to humans in efficacy studies concerned with short stature and underweight conditions. It has never been reported by doping control laboratories. Norbolethone was identified in two urine samples from one athlete by matching the mass spectra and chromatographic retention times with those of a reference standard. The samples also contained at least one likely metabolite. The samples were also unusual because the concentrations of endogenous steroids were exceptionally low. Since norbolethone is not known to be marketed by any pharmaceutical company, a clandestine source of norbolethone may exist. Copyright © 2002 John Wiley & Sons, Ltd. [source] | ||||||||||