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Test Mixture (test + mixture)
Selected AbstractsCyclodextrin-based nonaqueous electrokinetic chromatography with UV and mass spectrometric detection: Application to the impurity profiling of amiodarone,ELECTROPHORESIS, Issue 17 2008Roelof Mol Abstract The potential of nonaqueous electrokinetic chromatography (NAEKC) using cyclodextrins (CD) for the analysis of basic drugs and related compounds was evaluated. Both UV absorbance and mass spectrometric (MS) detection were employed. Addition of neutral CD to the NA background electrolyte did not significantly enhance the separation of a test mixture of basic drugs, and no change in selectivity was observed. In contrast, anionic single-isomer-sulfated CD strongly added to the selectivity of the NAEKC system inducing an improved resolution among the test compounds and increasing the migration time window. The applicability of the NAEKC system using anionic CD is demonstrated by the profiling of a sample of the drug amiodarone that had been stored for 1,year at room temperature. Amiodarone is poorly soluble in water. NAEKC-UV analysis indicated the presence of at least seven impurities in the amiodarone sample. In order to identify these compounds, the NAEKC system was coupled directly to electrospray ionization (ESI) ion-trap MS. The total of detected impurities increased to 12 due to the added sensitivity and selectivity of MS detection. Based on the acquired MS/MS data, three sample constituents could be identified as ,known' impurities (British Pharmacopoeia), whereas for three unknown impurities molecular structures could be proposed. Estimated limits of detection for amiodarone using the NAEKC method were 1,,g/mL with UV detection and 15,ng/mL with ESI-MS detection (full-scan). Based on relative responses, the impurity content of the stored drug substance was estimated to be 0.33 and 0.47% using NAEKC-UV and NAEKC-ESI-MS, respectively. [source] Phenotypic and genotypic characterization of competitive exclusion products for use in poultryJOURNAL OF APPLIED MICROBIOLOGY, Issue 6 2003R.D. Wagner Abstract Aims: Phenotypic and genotypic bacteria identification methods were compared for their efficacy in determining the composition of competitive exclusion (CE) products. Methods and Results: Phenotypic methods used for bacterial identification were fatty acid methyl ester profiles, biochemical assays and carbohydrate utilization profiles. Genotypic methods were MicroSeq16S rRNA sequence analysis and BLAST searches of the GenBank sequence database. Agreement between phenotypic and genotypic methods for identification of bacteria isolated from the Preempt CE product was 20%. A defined test mixture of bacteria was identified to the species level 100% by BLAST analysis, 64% by MicroSeq and 36% by phenotypic techniques. Conclusions: The wide range of facultative and obligate anaerobic bacteria present in a CE product are more accurately identified with 16S rRNA sequence analyses than with phenotypic identification techniques. Significance and Impact of the Study: These results will provide guidelines for manufacturers of CE products to submit more reliable product information for market approval by regulatory agencies. [source] High-performance separation of small inorganic anions on a methacrylate-based polymer monolith grafted with [2(methacryloyloxy)ethyl] trimethylammonium chlorideJOURNAL OF SEPARATION SCIENCE, JSS, Issue 15-16 2009Damian Connolly Abstract A glycidyl methacrylate- co -ethylene dimethacrylate monolith in capillary format (100 ,m/id) has been grafted with chains of poly([2(methacryloyloxy)ethyl] trimethylammonium chloride (poly-META) and applied to the ion-chromatographic separation of selected inorganic anions. Grafting chains of META onto the generic monolithic scaffold resulted in a monolith with ,electrolyte responsive flow permeability', which manifested as increased permeability in the presence of electrolyte solutions. Using an eluent of 2 mM sodium benzoate and on-column contactless conductivity detection, a test mixture of six common anions was isocratically separated and detected within 12 min, with the first four anions baseline resolved within a retention time window of 3.2 min. Retention time precision was ,1.2% for all anions tested. Separation efficiencies of 15 000 N/m were achieved for fluoride at 1 ,L/min, with column efficiencies up to 29 500 N/m obtained at a lower flow rate of 100 nL/min. Furthermore, repeatability of the column modification procedure using photografting methods was acceptable, with retention times between replicate columns matching within 9%. [source] Comparison of ethylammonium formate to methanol as a mobile-phase modifier for reversed-phase liquid chromatographyJOURNAL OF SEPARATION SCIENCE, JSS, Issue 5 2006Martin M. Waichigo Abstract Ethylammonium formate (EAF), (C2H5NH3+HCO2,), is a room-temperature ionic liquid that has a polarity similar to that of methanol (MeOH) or acetonitrile. The separation at 1 mL/min of a test mixture of vitamins or phenols on a polystyrene-divinylbenzene column using either an EAF- or MeOH-water mobile phase is similar in terms of both resolution and analysis time. Because the viscosity of EAF is higher than that of MeOH, the plate count for phenol at room temperature is lower by about a factor of 1.1,1.4 depending on the flow rate. However, van Deemter plots show that this loss in plate count at 1 mL/min can be recovered and improved from 1500 to 2400 plates by working at a slightly elevated temperature of 55°C. A slower flow rate such as 0.8 mL/min can also substantially improve the plate count as compared to 1,1.5 mL/min. Log P (octanol partition coefficient) versus log k, data for a variety of neutral test solutes are again similar whether EAF or MeOH is used as the organic modifier. Resolution of certain peak pairs such as 2,4-dinitrophenol/2,4,6-trinitrophenol and p -aminobenzoate/benzoate is enhanced using EAF as compared to MeOH. One advantage of EAF is that control of retention of solutes such as water-soluble vitamins under totally aqueous mobile phase conditions is environmentally preferable for quality control applications. In addition, EAF seems to be a milder mobile-phase modifier than MeOH for certain proteins such as lysozyme. [source] Mineralization of organic contaminants in sludge-soil mixturesENVIRONMENTAL TOXICOLOGY & CHEMISTRY, Issue 4 2001Bo Gejlsbjerg Abstract The mineralization of 14C-labeled linear alkylbenzene sulfonate (LAS), nonylphenol (NP), nonylphenol-di-ethoxylate (NP2EO), di-(2-ethylhexyl)phthalate (DEHP), pyrene, and 1,4-dichlorobenzene (DCB) was investigated in different sludge-soil mixtures and soils. Under aerobic conditions, the mineralization of LAS, NP, and NP2EO was between 50 and 81% of the added amounts after two months, while DEHP and pyrene were mineralized more slowly. The mineralization of the model chemicals was indirectly affected by the amount of sludge in the test mixtures. A higher content of sludge in the mixtures reduced the overall concentration of oxygen, which resulted in a decrease of the mineralization of several of the model chemicals. In sludge-soil mixtures with predominantly anaerobic conditions, the mineralization was slower for all of the chemicals with the exception of DEHP and DCB. The mineralization of DCB was enhanced in mixtures with a high sludge content. No pronounced difference in the mineralization of the model chemicals (except DEHP) was observed when the sludge was mixed with three different agricultural soils. [source] Preparation of a stationary phase with s -triazine ring embedded group for reversed phase high-performance LCJOURNAL OF SEPARATION SCIENCE, JSS, Issue 19 2010Yingyu Li Abstract This paper describes the synthesis and chromatographic evaluation of a new polar-embedded stationary phase, which utilized 2,4,6-trichloro-1,3,5-triazine as the spacer. The resulting materials were characterized by elemental analysis, IR, and solid-state 13C NMR. Empirical test mixtures were utilized to evaluate the column, and showed that it had good performance for basic compounds and high selectivity for polyaromatic hydrocarbons. Moreover, the novel stationary phase has unique property, especially in the separation of "homologous alkaloids" from natural products. [source] | ||||||||||