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      Spectrophotometric Determination of N-Acetyl-L-Cysteine and N-(2-Mercaptopropionyl)-Glycine in Pharmaceutical Preparations

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          Abstract

          A simple spectrophotometric method for the determination of N-acetyl-L-cysteine (NAC) and N-(2-mercaptopropionyl)glycine (MPG) in pharmaceutical preparations was developed, validated, and used. The proposed equilibrium method is based on a coupled two-step redox and complexation reaction. In the first step, Fe(III) is reduced to Fe(II) by NAC or MPG. Subsequently, Fe(II) is complexed with 2,4,6-tripyridyl-s-triazine (TPTZ). Several analytical parameters of the method were optimized for NAC and MPG analysis in the concentration range from 1.0  μM to 100.0  μM. Regression analysis of the calibration data showed a good correlation coefficient (0.9999). The detection limit of the method was 0.14  μM for NAC and 0.13  μM for MPG. The method was successfully applied to quantify NAC and MPG in pharmaceutical preparations. No interferences were observed from common pharmaceutical excipients.

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          Medical treatment of cystinuria: critical reappraisal of long-term results.

          We evaluated long-term results of a contemporary medical therapeutic regimen in patients with cystinuria and analyzed factors predictive of therapeutic success. A total of 27 adults with cystine urolithiasis were treated at our institution for 1.3 to 32 years (mean 11.6, overall 312 patient-years). We obtained data on the pre-referral period for 274 patient-years overall. Basic therapy included hyperdiuresis and alkalization. The thiols D-penicillamine or tiopronin were added when standard therapy failed to prevent new stones and stone growth or dissolve preexisting stones. X-ray and echography were performed every 4 months during the initial 2 years and every 6 months thereafter. In the pre-referral period 256 stone episodes occurred and 81 urological procedures were performed in 24 patients (0.93 and 0. 29 per patient-year, respectively). Nine patients were treated with added thiols. During the therapeutic period the incidence of stone episodes decreased to 66 (0.20 per patient-year, p <0.001), while the need for urological procedures decreased to 44 (0.14 per patient-year, p <0.001). No further urological procedures were required in 15 patients, including 4 treated with thiols. However, the remaining 12 patients, including 5 treated with thiols, underwent 1 to 7 procedures each (mean 0.26 per patient-year). In the 2 groups mean daily cystine excretion plus or minus standard deviation at baseline (863 +/- 253 versus 761 +/- 270 mg. daily) and mean urinary pH of about 7.4 did not differ significantly. However, daily urine volume was significantly higher in patients with arrested stone formation (3,151 +/- 587 versus 2,446 +/- 654 ml./24 hours, p = 0.006). Our study provides evidence that a regularly followed medical program based on high diuresis and alkalization with second line addition of thiols may arrest or markedly decrease cystine stone formation and preclude the need for urological procedures in more than half of the patients. However, patients poorly compliant with hyperdiuresis remain at risk for recurrence. We suggest that maintaining a daily urine volume of greater than 3 l. is essential for therapeutic success regardless of whether thiol derivatives are administered.
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            2,4,6-Tripyridyl-s-triazine as Reagent for Iron. Determination of Iron in Limestone, Silicates, and Refractories

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              Analysis of cysteine and N-acetylcysteine in human plasma by high-performance liquid chromatography at the basal state and after oral administration of N-acetylcysteine.

              A high-performance liquid chromatographic method for the determination of free reduced cysteine and N-acetylcysteine in human plasma at the basal state and after oral administration of N-acetylcysteine is described. The method is based on acid-catalysed conversion of plasma thiols to the corresponding S-nitroso derivatives by excess of nitrite and their subsequent cation-pairing RP-HPLC with detection at 333 nm. Recovery rates of cysteine and N-acetylcysteine added to human plasma were 94.6 and 99.6%, respectively. Inter- and intra-day precision were below 6%. In healthy humans (n = 5), free reduced cysteine was determined to be (mean+/-S.E.) 10.0+/-0.96 microM. No N-acetylcysteine was detected in plasma of these subjects above the limit of detection (e.g. 170 nM). The method was successfully applied to a pharmacokinetic study on orally administered N-acetylcysteine to healthy volunteers.
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                Author and article information

                Journal
                Int J Anal Chem
                IJAC
                International Journal of Analytical Chemistry
                Hindawi Publishing Corporation
                1687-8760
                1687-8779
                2011
                23 May 2011
                : 2011
                : 140756
                Affiliations
                Department of Analytical Chemistry, Faculty of Chemistry and Technology, University of Split, Teslina 10/V, 21000 Split, Croatia
                Author notes
                *Lea Kukoc-Modun: lkmodun@ 123456gmail.com

                Academic Editor: D. Tsikas

                Article
                10.1155/2011/140756
                3103845
                21647283
                1a6adf83-7923-4de4-bbe9-28f35fb10fac
                Copyright © 2011 L. Kukoc-Modun and N. Radić.

                This is an open access article distributed under the Creative Commons Attribution License, which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.

                History
                : 13 January 2011
                : 2 March 2011
                : 12 March 2011
                Categories
                Research Article

                Analytical chemistry
                Analytical chemistry

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