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《Analytical letters》2012,45(2):241-251
Abstract Biamperometric titration and differential pulse polarography (DPP) are described for the analysis of nomifensine maleate powder and commercial capsules (MeritalR -50 mg). The biamperometric method involved the titration in cold dil. HCl medium against 0.01 M - NaN02 and electrometric detection of end point. The mean percent recoveries obtained were 100.0 ± 0.87 and 99.2 ± 0.95 for the authentic powder and capsules, respectively. The DPP method was performed by measuring the peak current, iP, obtained from the recorded differential polarogram under constant 50mV modulation amplitude. The peak current was measured at the peak potential of ? 1.02 V on the dropping mercury electrode (DME) versus Ag/AgCl/KCl (sat.) reference electrode at pH 5.0 (acetate buffer). A linear relationship between peak current and concentration was demonstrated in the range 3 to 30μg ml?1. The mean percent recovery for the capsules was 103.1 ± 1.26. 相似文献
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Asensi-Bernardi L Martín-Biosca Y Sagrado S Medina-Hernández MJ 《Biomedical chromatography : BMC》2012,26(11):1357-1363
This report is the first evidence of enantioselective binding of nomifensine to human serum albumin (HSA) and plasma proteins. The overall process with HSA included: (i) consistent experimental design along two independent sessions; (ii) incubation of nomifensine–HSA designed mixtures; (iii) ultrafiltration for separating the unbound enantiomers fraction; (iv) electrokinetic chromatography (EKC) using heptakis‐2,3,6‐tri‐O‐methyl‐β‐cyclodextrin as chiral selector to provide experimental data for enantiomers (first, E1, and second, E2, eluted ones); and (v) a recent direct equation allowing univariate tests and robust statistics to provide consistent parameters and uncertainty. A significant enantioselectivity to HSA (2.7 ± 0.1) was encountered, related to a 1:1 stoichiometry and log affinity constants of 3.24 ± 0.10 and 3.67 ± 0.08 for E1 and E2, respectively. The protein binding (PB) estimated at physiological concentration levels was 40 ± 5 and 63 ± 4% for E1 and E2, respectively. The use of synthetic human sera allowed in vitro estimation of the total plasma PB for the racemate (61 ± 5%; coincident with in vivo values), and its enantiomers (58 ± 7 and 64 ± 4% for E1 and E2, respectively). Comparison allowed the relative importance of HSA respect to other plasma proteins for binding nomifensine to be established. Copyright © 2012 John Wiley & Sons, Ltd. 相似文献
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