Biomedical subjects

L T Taylor

Publications and source records attributed to L T Taylor.

47 records · Page 3Linked to original sources

PubMed1994

Use of supercritical fluid extraction for sample preparation of sustained-release felodipine tablets.

Supercritical fluid extraction (SFE) was shown to be an accurate and precise alternative to liquid extraction for sample preparation of sustained-release felodipine tablets (5 mg potency) while realizing an 80% reduction in solvent consumption. Extractions of felodipine spiked on an inert support were used to evaluate the solubility of felodipine in CO2 as well as analyte trapping after SFE. Even though the pure drug was found to be soluble in pure CO2, extractions of felodipine from the tablet matrix required moderate modifier concentrations [8.7% (v/v) methanol in CO2] in order to overcome strong matrix-drug interactions. Sequential static/dynamic extraction steps were also required to quantitatively recover the drug from the tablet matrix, indicating that the drug extraction was diffusion-limited. Average recoveries (n = 5) for the optimized SFE method were determined to be 4.93 mg felodipine tablet (98.6% claim) with an RSD of 1.2% versus those for the liquid extraction procedure (n = 5, 4.98 mg/tablet, 99.6% claim, 2.4% RSD). Similar levels of drug degradation (0.12% expressed as felodipine) were also obtained with both the traditional liquid extraction and with the SFE method.

Chromatography, High Pressure Liquid↗

PubMed1994

Analysis of felodipine by packed column supercritical fluid chromatography with electron capture and ultraviolet absorbance detection.

A reproducible and selective supercritical fluid chromatography (SFC) method was developed for the analysis of felodipine, a drug indicated for the treatment of hypertension. Methanol-modified carbon dioxide was employed as the SFC mobile phase with both electron capture detection (ECD) and multi-wavelength detection (MWD) being used simultaneously for analyte determination. Chromatography limit of detection (LOD) and limit of quantitation (LOQ), linear dynamic range (LDR) and injection precision were obtained in order to assess chromatographic and detector performance for both the SFC/MWD and SFC/ECD/MWD systems. The method was shown to be stability indicating since felodipine could be separated from its potential oxidative degradation product, H152/37, in under 6 min (felodipine k' = 2.44). Sample throughput was increased by 60% with the SFC assay vs LC. The optimized SFC method was shown to be equivalent to an existing LC/UV procedure for the analysis of a sustained-release tablet while realizing a 92% saving in disposable solvent waste. In order to achieve further solvent savings overall, supercritical fluid extraction (SFE) with 8% methanol-modified carbon dioxide as the extraction fluid was used to extract felodipine from a sustained-release tablet (as opposed to traditional solvent extraction). Comparable drug recoveries were obtained with SFE sample preparation technique when either SFC or LC extract analysis was utilized.

Chromatography, Liquid↗

PubMed1994

Analytical inverse supercritical fluid extraction of polar pharmaceutical compounds from cream and ointment matrices.

It has been shown that inverse supercritical fluid extraction (SFE) can be used to analytically isolate a polar analyte from its matrix even at low concentrations (0.016%). Inverse SFE has been shown to be successful not only for the semi-solid Neosporin ointments, but also for the semi-liquid Neosporin creams as well. The technique has been shown to be superior to solid-phase extraction in both cases and affords the analytical chemist a quicker and safer method of sample preparation of analytes from both creams and ointments.

Chemical Phenomena↗

PubMed1994

Quantitative analysis of a drug in an animal feed employing sample preparation by supercritical fluid extraction.

A pharmaceutical agent has been quantified in a rat feed matrix wherein sample preparation was achieved by supercritical fluid extraction. Spiking levels ranged from 0.0335% to 1.12%. Pure carbon dioxide, solid phase trapping on stainless steel with acetonitrile and liquid chromatographic assay yielded recoveries greater than 90% with relative standard deviations less than 5% in all cases except for the lowest spiking level. In this case recovery was 89.6% with an RSD of 9.6.

Animal Feed↗

PubMed1994

Extraction and detection of sulfamethazine in spray-dried milk.

Processes that reduce moisture content of fluid milk may result in a high concentration of animal drug residues that are undetectable in the fluid milk on the basis of the same weights. The objectives were to determine the amount of sulfamethazine in spray-dried milk powder manufactured from fluid milk contaminated with sulfamethazine and to determine the effectiveness of supercritical fluid extraction as a means to extract sulfamethazine from dry milk powder. Fluid whole (3.25% fat) and skim milks with sulfamethazine added at concentrations of 5, 10, and 100 ppb were spray-dried. Based on total solids, observed concentrations were 493 and 523 ppb in skim and whole dry milk powders, respectively, compared with fluid milk containing 100 ppb of sulfamethazine as determined by HPLC. The increase in sulfamethazine concentration from fluid to dry milk was also measured quantitatively by a microbial receptor assay and an ELISA. Poor recoveries and variability in data were possibly due to binding of sulfamethazine to undetermined milk components. Dry milk powder with measured concentrations of sulfamethazine was treated with supercritical CO2. Sulfamethazine was not detectable in the extracted dry milk powder by microbial receptor assay or ELISA.

Animals↗

PubMed1993

Feasibility of thiocarbamate pesticide analysis in apples by supercritical fluid extraction and high-performance liquid chromatography.

Supercritical fluid extraction produced comparable results with liquid-solid extraction for the analysis of several thiocarbamate pesticides from apples at the 2 ppm spike level. These results were achieved with a simple one-step extraction procedure. The use of diatomaceous earth (Celite, Supelco, Inc.; Bellefonte, PA) served to increase thiocarbamate recoveries by aiding in the immobilization of the aqueous component of the apple matrix. High-performance liquid chromatography coupled with ultraviolet absorbance detection (HPLC-UV) had the most viable means of quantitation when compared with micro-HPLC-sulfur chemiluminescence detection (SCD) and gas chromatography-flame-ionization detection (GC-FID). The small injection volumes used with the micro-HPLC-SCD system made thiocarbamate detection at a spiking level of 2 ppm impossible. SCD did provide, however, valuable qualitative information about the nature of the apple coextractants.

Chromatography, High Pressure Liquid↗

PubMed1993

Assessment of supercritical fluids for drug analysis.

Supercritical fluid (SF) CO2 is receiving a great deal of interest in the scientific and engineering community as a replacement for toxic organic solvents. Analytical chemists employ large quantities of organic solvents during preparation of the sample for analysis. The application of SF extraction with CO2 and modified CO2 to the isolation of active drug components and metabolites from various pharmaceutical and biological matrices is reviewed. Studies are described that deal with spiked drugs in animal feed, residual solvent in drug formulations, and active ingredients in over-the-counter products. The experimental challenges to implementing this technology for trace analysis are discussed. While much of the impetus for working with SFs is prompted by regulatory issues, it would appear that SFs afford the analyst a better-cheaper-faster-safer way of performing drug analysis.

Animal Feed↗

PubMed1992

Supercritical fluid extraction of active components in a drug formulation.

Sulfamethoxazole and trimethoprim have been extracted from a drug formulation, Septra Infusion, with pure supercritical carbon dioxide. Both direct extraction of the aqueous-based matrix and indirect extraction of the formulation immobilized onto Celite were studied. Exhaustive analytical extraction was achieved when active components were less than 1.0 mg. A number of co-extractants were found, but each was blind to the HPLC/UV assay.

Drug Combinations↗

PubMed1991

Collection efficiency of various solid-phase traps for off-line supercritical fluid extraction.

Solid-phase extraction tubes were evaluated as traps for off-line supercritical fluid extraction. Normal- and reversed-phase traps were studied with hydrocarbons, phenols, and a "test mixture" in order to determine the trapping efficiency. These traps were then used for the extraction of PCBs from river sediment. Polyethylene frits were also investigated for their use as solid-phase traps in SFE.

Polychlorinated Biphenyls↗

PubMed1989

Gradient separation of PTH-amino acids employing supercritical CO2 and modifiers.

Twenty-four PTH-amino acids are rapidly and efficiently separated on a packed cyanopropyl Zorbax column by gradient elution of supercritical CO2 and tetramethylammonium hydroxide-modified methanol. Complete or partial resolution of 22 derivatives is observed with only valine coeluting with norleucine and lysine coeluting with asparagine. A wide variety of stationary phases and modifiers are investigated with supercritical CO2 in attempting to achieve the separation in less than 15 min. Critical to achieving a rapid and efficient separation is the control of modifier flow into the CO2. No modifier is required for elution of neutral PTH-amino acids. The addition of base plays a major role in the elution of acidic and basic PTH-amino acids. Peak tailing is minimized and the elution order of several peaks is altered upon incorporation of reagent into the mobile phase.

Amino Acids↗

PubMedDate not supplied

Comparison of supercritical CHF3 and CO2 and methanol-modified CHF3 and CO2 for extraction of sulfonamides from chicken liver.

Supercritical CHF3 and methanol-modified CHF3 were compared with supercritical CO2 and methanol-modified CO2 for extraction of sulfonamides from fortified chicken liver admixed with Hydromatrix. Results showed that solvating power and selectivity were higher for supercritical and methanol-modified CHF3 than for supercritical and methanol-modified CO2. Visual observation showed that chicken liver extract obtained with methanol-modified CHF3 was cleaner than that obtained with methanol-modified CO2. Fat precipitated in the solvent trap when CO2 was used as the extraction medium. Also, simple off-line collection of fortified chicken liver extract obtained with CO2 in a solid-phase extraction cartridge (packed with either C18 or alumina) followed by phosphate buffer-methanol (50 + 50) rinse yielded an extract that required no further cleanup for analysis.

Animals↗