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Biomedical subjects

H M McNair

Publications and source records attributed to H M McNair.

10 recordsLinked to original sources

Effect of the eluent pH and acidic modifiers in high-performance liquid chromatography retention of basic analytes.

The retention of ionogenic bases in liquid chromatography is strongly dependent upon the pH of the mobile phase. Chromatographic behavior of a series of substituted aniline and pyridine basic compounds has been studied on C18 bonded silica using acetonitrile-water (10:90) as the eluent with different pHs and at various concentrations of the acidic modifier counter anions. The effect of different acidic modifiers on solute retention over a pH range from 1.3 to 8.6 was studied. Ionized basic compounds showed increased retention with a decrease of the mobile phase pH. This increase in retention was attributed to the interaction with counter anions of the acidic modifiers. The increase in retention is dependent on the nature of the counter anion and its concentration in the mobile phase. It was shown that altering the concentration of counter anion of the acidic modifier allows the optimization of the selectivity between basic compounds as well as for neutral and acidic compounds.

Buffers↗

Geometry of chemically modified silica.

The effect of alkyl chain length on adsorbent pore volume and void volume of HPLC columns is described. The results provide evidence that alkyl chains attached on silica surface are densely packed. A correlation of a decrease of pore volume with an increase of the alkyl modifier chain length was found. Effective molecular volume of bonded chains was found to be similar to the molecular volume of corresponding liquid alkanes. An absence of noticeable penetration of acetonitrile, methanol, or tetrahydrofuran molecules between bonded chains at any water-organic eluent composition was found.

Adsorption↗

Low-energy interactions in high-performance liquid chromatography.

Liquid chromatographic systems with very weak excessive analyte-adsorbent interactions have been studied. These systems consisted of a homologous series of n-alkanes as both analytes and mobile phases with a C18 reversed-phase adsorbent. A linear decrease of the analyte retention volume with an increase of the number of analyte carbon atoms was found. Corresponding increases of analyte retention with an increase in the number of eluent carbon atoms was also discovered. An explanation of these two effects on the basis of adsorption theory is proposed. A good correlation of column hold-up volume calculated by interpolation of the retention dependencies for above mentioned systems with that measured by the minor disturbance method has been shown. A study of the temperature dependencies of these alkane systems has shown entropy-governed retention dependencies.

Chromatography, High Pressure Liquid↗

Fast HPLC for the analysis of oxygen heterocyclic compounds of citrus essential oils.

A fast HPLC method for the determination of the oxygen heterocyclic compounds of citrus essential oils was developed. Five different oils were analyzed under identical conditions, by reversed-phase HPLC with photodiode array detector, for a direct comparison of the composition of their oxygen heterocyclic fraction. Analysis time was 7 min. The oils analyzed were lemon, bergamot, mandarin, sweet orange, and bitter orange. The method developed is good for rapid screening or fingerprinting of these essential oils; a slightly slower method is recommended for higher resolution and better quantitative results.

Chromatography, High Pressure Liquid↗

Biogenic amine survey and organoleptic changes in fresh, stored, and temperature-abused bluefish (Pomatomus saltatrix).

Changes in histamine, putrescine, and cadaverine concentrations in bluefish filets (Pomatomus saltatrix) stored at 5, 10, and 15 degrees C were determined using high-performance liquid chromatography. An organoleptic assessment was conducted simultaneously with the biogenic amine analyses. The histamine levels found in fresh bluefish obtained from wholesale seafood distributors ranged between <1 ppm and 99 with an average of 39 ppm. Putrescine and cadaverine were not found in fresh bluefish. Fish fillets stored at each of the three temperatures developed histamine. The greatest accumulation of histamine was observed in fish stored at 15 degrees C, which developed histamine levels as high as 2,200 ppm. Putrescine levels increased at each temperature during storage. Cadaverine was present only in uninoculated bluefish stored at 15 degrees C. Histamine achieved higher levels in bluefish pieces inoculated with Morganella morganii, which demonstrates that bluefish support bacterial histamine formation. Histamine levels at each temperature exceeded the 50-ppm advisory level established by the Food and Drug Administration before 100% sensory rejection. Standard plate counts increased during storage of fish at all temperatures, but the correlation between histamine levels and standard plate count was not significant.

Animals↗

Separation and quantification of the B6 vitamers in plasma and 4-pyridoxic acid in urine of adolescent girls by reversed-phase high-performance liquid chromatography.

The vitamin B6 status of seemingly healthy adolescent girls was determined using several accepted and proposed parameters in an effort to establish guidelines for status evaluation. High-performance liquid chromatography-derived plasma B6 vitamers (pyridoxal phosphate, PLP; pyridoxine phosphate. PNP; pyridoxamine phosphate, PMP; pyridoxal, PL; pyridoxine, PN; and pyridoxamine, PM) and 4-pyridoxic acid (4-PA) concentrations and urinary 4-PA levels of 28 white adolescent females, 12-15 years, having radiomonitored plasma PLP concentrations and coenzyme stimulation of erythrocyte alanine aminotransferase activities indicative of adequate status were determined. Mean vitamin B6 and protein intakes were 1.48 mg and 78.3 g. Ranges for plasma B6 vitamer and 4-PA concentrations (nmol/l) were: PLP, 40.9-122.2; PNP, non-detectable (ND)-16.1; PMP, ND-8.1; PL, ND-15; PN, ND-21.9; PM, ND-17.8; and 4-PA, ND-55.7. PLP was the only vitamer found in plasma of all subjects. Urinary 4-PA concentrations ranged from 0.11 to 2.50 mumol/mmol of creatinine. B6 vitamer values of these girls should be of use in the establishment of normal ranges for vitamin B6 status parameters.

Adolescent↗

Plasma B6 vitamer and 4-pyridoxic acid concentrations of men fed controlled diets.

A rapid and sensitive procedure is described for the analysis of all the B6 vitamers and 4-pyridoxic acid in human plasma utilizing reversed-phase high-performance liquid chromatography with ultraviolet and fluorometric detection. Pyridoxal phosphate values obtained by radiometric and chromatographic, ultraviolet and fluorometric, assays were highly correlated as were pyridoxine phosphate values determined using both detectors. Plasma B6 vitamer and 4-pyridoxic acid concentrations of 22 men fed diets containing 0.75-0.98 mg of vitamin B6 daily for eight weeks were in the range of reported values; pyridoxal phosphate was their predominant plasma B6 vitamer. This methodology should be useful in the assessment of vitamin B6 requirements.

Adult↗

High-pressure liquid-chromatographic assay of nucleotide-pool concentrations during polysaccharide biosynthesis in four ascomycetes.

High-resolution liquid-chromatographic methods developed for analyzing nucleotide pools at the nanogram level in four representative species of ascomycetes (Penicillium citrinum, Aspergillus niger, Fusarium moniliforme, and Cladosporium herbarum) were used to study polysaccharide biosynthesis. Nucleotides extracted from the mycelial mat were preseparated from interfering polysaccharides, glycoproteins, and nucleic acids on a column of Biogel P-2. Resolution of 18 nucleotides from each fungal species was accomplished on AS-Pellionex-SAX, pellicular anion-exchanger by using a high-pressure liquid chromatograph. Nucleotides were identified by comparing peak retention-times, by differential u.v. absorption with two detectors in series at selected wavelengths, and by acid or enzymic hydrolysis with product identification by liquid chromatography. Pyrimidine bases exceeded purines by at least three fold, and uridine nucleotides often constituted 60-80 mole percent of the total nucleotides; extractable cytidine nucleotides were negligible. Uridine 5'-(2-acetamido-2-deoxy-alpha-D-glucopyranosyl disphosphate) is the preponderant nucleotide throughout the growth cycles of all four species, amounting to 30-60% of all nucleotides present. For all four fungal species, a burst of nucleotide formation was observed after the first 48h (15-30 mumol/g tissue), with fluctuations that eventually fell to 0.1 mumol/g on the tenth day.

Ascomycota↗

Polyamides (nylon) composition analysis by capillary zone electrophoresis.

A new and simple method of analysis for polyamide composition is described. Polymer samples were decomposed to their corresponding monomers by hydrobromic acid (HBr) and the decomposed products were analyzed by capillary zone electrophoresis (CZE). Amines from polyamides were derivatized with fluorescamine and detected by UV at 280 nm. Aliphatic acids were detected by direct UV at 205 nm. Sample treatment is much simpler than published methods, and electropherograms show a good separation of decomposed products under the proper conditions.

Electrophoresis, Capillary↗