Simultaneous Determination of Chlorinated and Brominated Acetic Acids in Various Environmental Water Matrixes by High-Performance Liquid Chromatography-Inductively Coupled Plasma Tandem Mass Spectrometry without Sample Preparation.

The halogenated acetic acids (HAAs) are generally considered as environmental contaminants and are suspected to pose a major public health concern. The inductively coupled plasma mass spectrometry (ICPMS) has been improved by coupling with the tandem mass spectrometry technology (ICPMS/MS), enabling ultratrace determination of heteroatoms. There have been few reports about the determination of chlorine-containing analytes by high-performance liquid chromatography (HPLC)-ICPMS/MS but none about utilizing this technique for the speciation analysis of organic halogenated compounds in environmental matrixes. We report a rapid method for the simultaneous determination of up to nine chlorinated and brominated acetic acids by HPLC-ICPMS/MS in Austrian surface, ground, and tap water. The chromatographic separation of the main five regulated haloacetic acids (so-called HAA5: chloroacetic acid, dichloroacetic acid, trichloroacetic acid, bromoacetic acid, and dibromoacetic acid) could be achieved in <6 min with limits of detection of 1.4-1.6 µg Cl L-1 and 0.8-1.5 µg Br L-1 for the chlorinated and brominated acetic acids, respectively. The method was validated through recovery experiments at four concentration levels (10-500 µg L-1) as well as by analyzing the U.S. Environmental Protection Agency (EPA) 552.2 CRM (certified reference material) in pure water and in three different water matrixes (tap, river, and groundwater), and thereby validated for repeatability (RSD% 1-10%), accuracy (±1.0-15%), and linearity (r2 = 0.9996-0.9999). The method fulfills the regulatory concentration limits by the EPA for HAA5 [maximum contaminant level (MCL) 60 µg L-1] and the limits currently being reviewed by the European Union for HAA9 (80 µg L-1) and demonstrates the advantages of HPLC-ICPMS/MS for the analysis of environmental water samples for halogen-tagged contaminants.

Novel montelukast sodium-loaded stable oral suspension bioequivalent to the commercial granules in rats.

To develop a montelukast sodium-loaded stable oral suspension bioequivalent to the commercial granules in rats, several montelukast sodium-loaded suspensions were prepared with a suspending agent, stabilizers and anti-aggregation agents, and their stabilities were investigated by visually observing the sedimentation phenomenon and determining the concentration of the degradation product. Moreover, dissolution and pharmacokinetic studies of the optimized formulation were examined in rats compared to commercial montelukast sodium-loaded granules. Avicel RC-591 (Avicel), a suspending agent, prevented the sedimentation of these suspensions at >2.496 (w/v) per cent composition. Amongst the stabilizers tested, fumaric acid provided the lowest concentration of montelukast sulphoxide (a degradation product) in these suspensions at 40 °C, demonstrating its excellent stabilizing activity. Furthermore, as an anti-aggregation agent, glycerin gave lower amounts of degradation product than those with poloxamer 407 and Tween 80. In particular, montelukast-loaded oral suspension, an aqueous suspension containing montelukast sodium/Avicel/fumaric acid/glycerin at a concentration of 312/2496/15.6/62.4 (mg/100 ml), and the commercial granules exhibited similar dissolution profiles in 0.5% (w/v) aqueous solution of sodium lauryl sulphate. Moreover, the pharmacokinetics in rats provided by this suspension was comparable to that of the commercial granules, suggesting that they were bioequivalent. In addition, it was physically and chemically stable at 40 °C for at least 6 months. Thus, this montelukast sodium-loaded oral suspension, with bioequivalence to the commercial granules and excellent stability, could be a prospective dosage form for the treatment of asthma.

Multi-analyte quantification in bioprocesses by Fourier-transform-infrared spectroscopy by partial least squares regression and multivariate curve resolution.

This paper presents the quantification of Penicillin V and phenoxyacetic acid, a precursor, inline during Pencillium chrysogenum fermentations by FTIR spectroscopy and partial least squares (PLS) regression and multivariate curve resolution - alternating least squares (MCR-ALS). First, the applicability of an attenuated total reflection FTIR fiber optic probe was assessed offline by measuring standards of the analytes of interest and investigating matrix effects of the fermentation broth. Then measurements were performed inline during four fed-batch fermentations with online HPLC for the determination of Penicillin V and phenoxyacetic acid as reference analysis. PLS and MCR-ALS models were built using these data and validated by comparison of single analyte spectra with the selectivity ratio of the PLS models and the extracted spectral traces of the MCR-ALS models, respectively. The achieved root mean square errors of cross-validation for the PLS regressions were 0.22 g L(-1) for Penicillin V and 0.32 g L(-1) for phenoxyacetic acid and the root mean square errors of prediction for MCR-ALS were 0.23 g L(-1) for Penicillin V and 0.15 g L(-1) for phenoxyacetic acid. A general work-flow for building and assessing chemometric regression models for the quantification of multiple analytes in bioprocesses by FTIR spectroscopy is given.

Management of hyperphosphataemia in chronic kidney disease: summary of National Institute for Health and Clinical Excellence (NICE) guideline.

Bone disease and ectopic calcification are the two main consequences of hyperphosphataemia of chronic kidney disease (CKD). Observational studies have demonstrated that hyperphosphataemia in CKD is associated with increased mortality. Furthermore, the use of phosphate binders in dialysis patients is associated with significantly lower mortality. The UK Renal Registry data show significant underachievement of phosphate targets in dialysis patients. It is believed to be due to wide variation in how management interventions are used. The National Institute for Health and Clinical Excellence (NICE) has developed a guideline on the management of hyperphosphataemia in CKD. This is based on the evidence currently available using the Grading of Recommendations Assessment, Development and Evaluation (GRADE) methodology. This review outlines the recommendations including research recommendations and discusses methodology, rationale and challenges faced in developing this guideline and the health economic model used to assess the cost-effectiveness of different phosphate binders.

Fully automated synthesis of ¹¹C-acetate as tumor PET tracer by simple modified solid-phase extraction purification.

INTRODUCTION: Automated synthesis of (11)C-acetate ((11)C-AC) as the most commonly used radioactive fatty acid tracer is performed by a simple, rapid, and modified solid-phase extraction (SPE) purification. METHODS: Automated synthesis of (11)C-AC was implemented by carboxylation reaction of MeMgBr on a polyethylene Teflon loop ring with (11)C-CO2, followed by acidic hydrolysis with acid and SCX cartridge, and purification on SCX, AG11A8 and C18 SPE cartridges using a commercially available (11)C-tracer synthesizer. Quality control test and animals positron emission tomography (PET) imaging were also carried out. RESULTS: A high and reproducible decay-uncorrected radiochemical yield of (41.0 ± 4.6)% (n=10) was obtained from (11)C-CO2 within the whole synthesis time about 8 min. The radiochemical purity of (11)C-AC was over 95% by high-performance liquid chromatography (HPLC) analysis. Quality control test and PET imaging showed that (11)C-AC injection produced by the simple SPE procedure was safe and efficient, and was in agreement with the current Chinese radiopharmaceutical quality control guidelines. CONCLUSION: The novel, simple, and rapid method is readily adapted to the fully automated synthesis of (11)C-AC on several existing commercial synthesis module. The method can be used routinely to produce (11)C-AC for preclinical and clinical studies with PET imaging.

In vitro function of buffy coat-derived platelet concentrates stored for 9 days in CompoSol, PASII or 100% plasma in three different storage bags.

BACKGROUND AND OBJECTIVES: The aim of the study was to compare the in vitro quality of buffy coat-derived platelet concentrates (PC) during extended storage in plasma or additive solution in three different storage bags. MATERIALS AND METHODS: A pooled and split design was chosen so that identical PCs were produced in either 100% plasma, 70% PASII : 30% plasma or 70% CompoSol : 30% plasma (n = 6 each). This was repeated for three different manufacturers' platelet storage bags (Fresenius, Baxter and Pall). PCs were sampled on days 1, 5, 7 and 9 of storage and tested in vitro using a variety of tests of platelet function. For each bag type, storage in PASII or Composol was compared with plasma (data taken across the entire storage period), and differences occurring with time were analysed for all storage media. RESULTS: The pH of all PCs was > 6.8 at day 9 of storage. In vitro platelet function, as assessed by markers of platelet activation and metabolism, of PCs stored in CompoSol appeared to be similar to that of PCs stored in plasma over 9 days of storage. In contrast, PCs stored in PASII tended to have significantly higher levels of platelet activation (almost a twofold increase in % platelets positive for CD62P by day 5) and lower hypotonic shock response (approximately 40%, by day 7) compared to either PCs stored in 100% plasma or 70% CompoSol. The magnitude of the differences observed between platelet storage media appeared to be dependent on the type of platelet storage bag with the highest degree of platelet activation and lowest hypotonic shock response values being observed in Fresenius bags in combination with PASII. CONCLUSIONS: The maintenance of platelet function in vitro during extended storage of PCs in platelet additive solutions is dependent on the combination of type of additive solution and type of platelet storage bag. For all bag types studied, storage in PASII resulted in poorer platelet function in vitro.

Rapid synthesis of partially O-methylated alditol acetate standards for GC-MS: some relative activities of hydroxyl groups of methyl glycopyranosides on Purdie methylation.

Mixtures containing the majority of partially O-methylated alditol acetates (PMAAs), necessary for the GC-MS based identification of glycosidic linkages in oligo- and polymeric structures were prepared. Rha, Fuc, Rib, Ara, Xyl, Man, Gal, and Glc were converted to their Me glycosides, and the products were progressively O-methylated using the Purdie reagent at 25 degrees C. Resulting PMGs were assayed by TLC and at times that were optimum for formation of mono-O-methyl derivatives and later for higher degrees of methylation; they were converted to PMAAs, in a process incorporating NaB(2)H(4) reduction. The majority of these can be used as standards for simultaneous identification of pyranosides and some furanosyl units particularly in heteropolysaccharides. The relative reactivities of OH-groups were determined by GC-MS as: Me alpha- and beta-Glcp, HO-2>HO-4>HO-3>HO-6, Me alpha- and beta-Galp, HO-3>HO-2>HO-4>HO-6, Me alpha-Manp, HO-3>HO-2>HO-4>HO-6, Me beta-Manp, HO-3>HO-4HO-6>HO-2, Me alpha-Rhap, OH-3>OH-2>OH-4; Me alphabeta-Fucp, OH-2>OH-3>OH-4, and Me alphabeta-Xylp, OH-2>OH-4>OH-3. The results differ from those obtained with Haworth, Hakomori, and Ciucanu methylation techniques, although some similarities occurred with the more rapid Kuhn method.

Determination of major compounds in sweet wines by headspace solid-phase microextraction and gas chromatography.

Headspace solid-phase microextraction (HS-SPME) was studied by high resolution gas chromatographic analysis of major compounds (ethyl acetate, methanol, 1-butanol, 2-butanol, 1-propanol, isobutanol, 2-methyl-1-butanol and 3-methyl-1-butanol) in sweet wines. Five different SPME fibres were tested and the influence of different factors such as temperature and time of desorption, extraction time, stirring, sample and vial volume, sugar and ethanol content were studied and optimized using model solutions. The SPME method was validated with the direct injection method. The proposed HS-SPME-GC method is an appropriate technique for the quantitative analysis of the mentioned analytes in real sweet wines.

Plasma glucose turnover and oxidation during hemodialysis: nutritional effect of dialysis fluid.

Mass transfer of glucose from dialysis fluid into patients is a source of energy and a form of nutrition during hemodialysis. The effect of glucose mass transfer on endogenous glucose metabolism and the overall nutritional importance of glucose transfer is not known. Rates of plasma glucose turnover and oxidation were determined by radioisotope-dilution techniques in patients with chronic renal failure (CRF) in the basal state, during hemodialysis, and during the infusion of glucose at a rate similar to the mass transfer rate (Mt: 6.6 +/- 0.7 mumol.min-1.kg-1). Rates of plasma glucose turnover (11.8 +/- 0.8 mumol.min-1.kg-1) and oxidation (4.0 +/- 0.4 mumol.min-1.kg-1) and contribution of glucose oxidation to the metabolic rate were similar to those of control subjects both in the basal state and during glucose infusion. During hemodialysis with acetate and glucose, the plasma glucose turnover rate was similar to that in the basal state, but the energy from glucose oxidation was less (P < or = 0.02) even though energy expenditure was increased by 21%. Immediate oxidation of plasma glucose and acetate accounted for 65% of the patients' energy expenditure. Energy (1172 kJ) from acetate Mt and glucose Mt surpassed the patients' energy requirements, offsetting the utilization of endogenous fuels, a sparing effect equivalent to 31 g fat or 70 g carbohydrate. Rates of plasma glucose turnover and oxidation during bicarbonate-glucose and glucose-free acetate hemodialysis were similar to that during acetate-glucose hemodialysis. However, without glucose or acetate in the bath fluid, a deficit as much as 669 kJ must be met by the oxidation of endogenous fuels. Addition of organic nutrients that supply energy to dialysis fluids may over time be a beneficial supplemental treatment for the malnutrition and body wasting commonly observed in CRF.

Control of predialytic hyperphosphatemia by oral calcium acetate and calcium carbonate. Comparable efficacy for half the dose of elemental calcium given as acetate without lower incidence of hypercalcemia.

Since Mai et al. found, with the intestinal lavage technique, that the same dose of elemental calcium given as acetate (Ca Ac) complexed in the gut of uremic patients twice as much phosphate as calcium carbonate (CaCO3) while inducing a rather low calcium absorption, we wanted to see if half the dose of elemental calcium given as Ca Ac could control, on medium term, the predialysis plasma phosphate as well as CaCO3 while inducing less frequent hypercalcemia. This was evaluated in a cross-over study of 3 periods of 10 weeks according to the sequence Ca Ac, CaCO3 and Ca Ac, in 12 compliant patients on chronic dialysis previously treated by CaCO3. Because of poor tolerance of Ca Ac during the first period, 4 patients were excluded and the results were assessed only on the 8 patients who completed the study. For half the doses of elemental calcium (620 +/- 250 mg versus 1,310 +/- 560 mg versus 710 +/- 200 mg/day), Ca Ac allowed the same control of predialytic hyperphosphatemia (1.67 +/- 0.34; 1.74 +/- 0.32; 1.75 +/- 0.38) with paradoxically comparable normal mean plasma calcium concentration (2.61 +/- 0.14; 2.56 +/- 0.13; 2.55 +/- 0.14 mmol/l). Plasma alkaline phosphatases and intact PTH concentrations remained also stable during the 3 periods. The frequency of hypercalcemia greater than 2.75 mmol/l (12; 9; 20%) and of hyperphosphatemia greater than 2 mmol/l (17; 22; 27%) were comparable with the 2 treatments. In conclusion, Ca Ac controls predialytic hyperphosphatemia as efficiently as CaCO3 for half the dose of elemental calcium without, however, decreasing the frequency of hypercalcemia.(ABSTRACT TRUNCATED AT 250 WORDS)

[Working conditions and health status of workers engaged in the production of zinc compounds]. / Usloviia truda i sostoianie zdorov'ia rabochikh, zaniatykh v proizvodstve soedinenii tsinka.

It was established that industrial shops engaged in zinc compounds' processing were characterized by considerable temperature shifts, relative humidity and air motion changes. In drying and packing shops, concentrations of the final product dusts were established at 0.8-2 mg/m3. The major occupational pathology was constituted by skin and upper respiratory tract diseases, including allergic and contact dermatitis, chronic pharyngitis, tonsillitis and rhinitis. Blood tests revealed B-lymphocytes: increases, circulating immune complexes and considerable levels of lymphocytic spontaneous blastotransformations. Erythrocytic acidic hemolysis was markedly changed, which proved disbalances in the system of red blood.

Improvements in the thin-layer chromatography of natural products. I. Thin-layer chromatography of the aflatoxins.

During the period which has elapsed since the aflatoxins were first isolated, one of the main problems has been the separation of the individual aflatoxins in pure form from aflatoxin-containing extracts. This separation has been best effected by thin-layer chromatography, and in this paper we describe how some of the difficulties may be overcome by using an appropriate combination of solvent system and silica gel preparation. For the examination of aflatoxin-containing extracts from the mycelia of Aspergillus flavus moulds, an initial freeze-drying step has been found to improve appreciably the quality of the chromatograms obtained.