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D C Locke

Publications and source records attributed to D C Locke.

11 recordsLinked to original sources

Separation of the eleven priority pollutant phenols by capillary zone electrophoresis.

Capillary zone electrophoresis (CZE) provides highly efficient separation of the eleven US EPA priority pollutant phenols. All of these phenols are completely resolved in fewer than 15 min in a 100 cm x 75 microns I.D. uncoated fused-silica capillary at 22.5 kV using a pH 9.8 phosphate-borate buffer. Buffer pH is the most critical parameter controlling resolution and separation time. A simple theoretical treatment greatly simplifies the pH optimization procedure. The effects on the separation of buffer concentration, applied voltage, and sample quantity injected were studied. Good calibration data were obtained for phenol concentrations up to 50 mg/l. Limits of detection for all phenols were less than 1 ppm.

Buffers

Design of a photoionization detector for high-performance liquid chromatography using an automated liquid-to-vapor phase interface and application to phenobarbital in an animal feed and to amantadine.

An automated liquid-to-vapor phase interface system forms the basis for a new high-performance liquid chromatography (HPLC)-photoionization detection (PID) system. The system incorporates a six-valve interface enabling peak trapping, solvent switching and thermal desorption of the solute of interest into a vapor phase PID. For reversed-phase HPLC, the eluted solute peak is isolated on a Tenax trap after dilution of the effluent with water; the water is then evaporated, following which the trapped solute is flash-evaporated into the PID system. For normal-phase HPLC, the column effluent is diluted with hexane, the solute peak is concentrated on a short column packed with a propyl-amino/cyano bonded phase and the solvent is evaporated. The solute is then eluted with water onto the Tenax trap, and the above procedure for reversed-phase HPLC followed. All operations are controlled with a microcomputer. The advantages of the new detector system include completely automated operation, fast sample preparation, high sensitivity, and inherent selectivity. The system was applied to phenobarbital, which was extracted with acetonitrile from spiked laboratory animal feed, and to amantadine. The phenobarbital assay used a normal-phase separation with hexane-methyl tert.-butyl ether-methanol eluent. The manual sample preparation time was 5 min and the limit of detection was 2 ng phenobarbital injected; a conventional HPLC assay with UV detection required a longer sample preparation time and had a detection limit of 700 ng. Amantadine was assayed using a reversed-phase HPLC system with a water-methanol-triethylamine-orthophosphoric acid mobile phase. The detection limit was 25 ng injected.

Amantadine

Determination of menadione in an animal feed using supercritical fluid extraction and HPLC with electrochemical detector.

Menadione (vitamin K3) is extracted from spiked rat chow using supercritical fluid carbon dioxide at 8000 psi and 60 degrees C. Quantitative extraction requires only 20 min. The extraction does not suffer from the problems associated with conventional solvent extraction of lipophilic materials from animal feeds. Menadione is determined in the extract, which does not require further cleanup, using reversed-phase high-performance liquid chromatography (HPLC) with reductive mode electrochemical detection at a silver electrode at -0.75 V vs. calomel. The minimum detectable quantity by the detector is 125 pg of menadione, and the response is linear over at least 4 orders of magnitude; however, the minimum quantity extractable is about 20 micrograms/g of feed. Repetitive extracts of a spiked feed sample over a five-day period show an average recovery of 90.5% with a relative standard deviation of 2.2% at the 1 mg/g level.

Animal Feed

Separation of aza-arenes by high-pressure liquid chromatography.

Fast, efficient liquid chromatographic separations of aza-arenes were obtained using both, reversed-phase, and adsorbent packings. Aza-arenes with 2-5 rings are separated within 20 minutes. Sample recovery is quantitative and permits subsequent uv and fluorescence spectrophotometric identifications. The detection limit for most aza-arenes was 1 ng with a 254-nm uv detector. An application to an air pollution problem demonstrates the usefulness of this approach.

Air Pollution

Determination of vitamin K1 in powdered infant formulas, using supercritical fluid extraction and liquid chromatography with electrochemical detection.

Vitamin K1 (phylloquinone) is extracted from commercial soy protein-based and milk-based powdered infant formulas by using supercritical fluid extraction with CO2 at 8000 psi and 60 degrees C. Quantitative extraction requires only 15 min, and does not suffer from the problems associated with conventional solvent extraction of lipophilic materials from media such as formulas. Vitamin K1 is determined in the extracts by using reverse-phase liquid chromatography (LC) with reductive mode electrochemical detection at a silver electrode polarized at -1.1 V vs SCE. LC run time is 9 min. The minimum detectable quantity is 80 pg, and response is linear over at least 5 orders of magnitude. Recovery of vitamin K1 from a milk-based powdered formula was 95.6% with RSD of 7.4%, and from a soy protein-based product, 94.4% recovery with RSD of 6.5%.

Adsorption

Liquid chromatographic determination of benzoyl peroxide in acne preparations.

A rapid, precise, and accurate liquid chromatographic (LC) method is described for the determination of benzoyl peroxide (BP) in acne preparations. BP is extracted from a water dispersion of the preparation with dichloromethane (DCM), and an aliquot is eluted from a C-18 reverse phase LC column with acetonitrile-0.10 M aqueous NaClO4. Selective and sensitive quantitation is accomplished with a reductive mode electrochemical detector. This detector is an order of magnitude more sensitive than a 240 nm UV absorption detector; the lower limit of detection is 2 ng for a 4 microL injection. The recovery of BP is 99.4% and the detector response is linear to at least 2 micrograms per 4 microL injection.

Acne Vulgaris