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PubMed1992

Determination of tetracyclines in bovine and porcine muscle by high-performance liquid chromatography using solid-phase extraction.

A method is presented for the determination of the three tetracyclines oxytetracycline, tetracycline and chlortetracycline in muscle, spiked at 100 ng/g, using high-performance liquid chromatography (HPLC). The concentration and extraction steps are carried out using Waters Environmental Sep-Pak cartridges. The principal steps involve homogenizing the sample in EDTA-McIlvaine buffer followed by centrifugation and precipitation of the supernatant using trichloroacetic acid. After further filtration and concentration on a Sep-Pak cartridge, the sample is eluted and analysed by HPLC with UV detection and confirmation by diode-array. The column used is a Nova-Pak C18 (4 microns) cartridge (10 cm x 8 mm I.D.). A phosphate-citrate-acetonitrile buffer, utilizing ion suppression, is the mobile phase. The analytes are detectable at levels down to 10 ng/g. The analyte identity can be confirmed at 20 ng/g by the use of diode-array detection and spectral library comparison.

Animals↗
PubMed1992

Ultramicrodetermination of cyanocobalamin in elemental diet by solid-phase extraction and high-performance liquid chromatography with visible detection.

The ultramicrodetermination of cyanocobalamin (9 ng/g) in elemental diet containing 46 kinds of compounds, with concentrations at least 50-10(6) times higher than that of cyanocobalamin, was performed by Sep-Pak C(18) purification and concentration of cyanocobalamin followed by HPLC with detection at 550 nm. The method is simple, rapid, sensitive and reproducible. The calibration graph was linear in the range of 0-0.2 micrograms. The recovery of cyanocobalamin was over 95% by the standard addition method. There was good agreement between the cyanocobalamin concentrations indicated and found.

Chromatography, High Pressure Liquid↗
PubMed1994

Determination of tetracycline antibiotics in animal tissues of food-producing animals by high-performance liquid chromatography using solid-phase extraction.

A high-performance liquid chromatographic (HPLC) method was developed for the determination of oxytetracycline (OTC), tetracycline (TC) and chlortetracycline (CTC) residues in bovine and porcine muscles. The method involved the homogenization of the sample in EDTA-McIlvaine buffer with added n-hexane and dichloromethane, centrifugation, precipitation of the supernatant using trichloroacetic acid and filtration. Preconcentration on Separcol SI C18 cartridges improved the clean-up and the recovery of tetracyclines that were separated by HPLC using the optimized mobile phase of 0.01 M oxalic acid-acetonitrile-methanol (45:35:20) on a Spherisorb ODS 2 column (250 x 4 mm I.D.). UV detection at 360 nm was applied with a detection limit of about 50 ng/g. The diode-array spectra confirmed the applicability of this method to the study of tetracycline residues in carcasses.

Animals↗
PubMed1995

Masking as a mechanism for evaporative loss of trace analyte, especially after solid-phase extraction.

Using a Pasteur pipette plugged with silanized glass wool and packed with C18-silica particles, we attempted to remove K2CO3 from an aqueous acetonitrile solution. In spite of extensive washing of the column with water after the sample was applied, elution with acetonitrile followed by evaporation gave a visible, white residue. It was found that the residue was derived from both the sample and the packing, including particles from the latter. Substitution of a plastic column/polyethylene frit for the Pasteur pipette/glass wool gave a more consistent residue, apparently because this improved the retention of particles. Subsequent experiments were conducted in the plastic hardware. The amount of the residue was observed to vary as much as 19-fold when C18-silica particles were tested from different manufacturers, and the residue could be reduced in amount as much as 9-fold when a column was prepared in the laboratory vs. the use of a comparable, pre-packed column. The water itself contributed some of the residue: even the "purest" water routinely available left a visible residue when 1.0 ml was appropriately evaporated (e.g. on Saran Wrap in a microwave oven). The recovery of an arbitrary trace analyte and internal standard (pentafluorobenzylated nucleobases at the low pg level) was 32% less when they were evaporated in acetonitrile that had been passed through an acetonitrile and water-washed cartridge containing C18-Si vs. evaporation in untreated acetonitrile. Collectively these results reveal that an evaporation can risk some loss of an analyte from masking by even subtle solvent contaminants.(ABSTRACT TRUNCATED AT 250 WORDS)

Acetonitriles↗
PubMed1989

A new method using simple solid phase extraction for the rapid gas-chromatographic mass-spectrometric determination of 11-dehydro-thromboxane B2 in urine.

A new gas-chromatographic mass-spectrometric method for the rapid determination of 11-dehydro-thromboxane B2 in urine, the major metabolite of systemic thromboxane formation, has been developed. Excellent sample clean-up was obtained in a single step by adsorption of 11-dehydro-TXB2 on phenylboronate cartridges, vigorous polar and organic washing and elution with an acidic methanol mixture. Then the pentafluorobenzylester trimethylsilylether derivative of 11-dehydro-TXB2 was formed and quantified in isotope dilution technique by negative chemical ionisation gas-chromatography tandem mass-spectrometry. The daughter fragments m/z 243/247 of the parent ion m/z 511/515 were monitored. Recovery was linear and quantitative over a wide range, accuracy was 95 + 7% and precision was 11% down to the very low pg range in biologic samples. Independent validation of this very fast extraction method with a reference method applying extensive sample purification with consecutive reversed and straight phase extraction, precolumn derivatisation, reversed phase high pressure liquid chromatography and tandem gas-chromatography mass-spectrometry gave excellent agreement of values. Values for 11-dehydro-TXB2 excretion in 8 healthy controls were 501 + 298 (range 231 to 1141) ng/g creatinin. Excretion was suppressed by aspirin, moderately elevated in heavy smokers (range 680 to 1540) and increased in patients with venous thrombosis or pulmonary embolism (2370 to 13350 ng/g creatinin). This rapid extraction method is useful for the highly specific and sensitive determination of 11-dehydro-TXB2 in large sample numbers.

Chromatography, High Pressure Liquid↗
PubMed1987

Solid-phase extraction and high-performance liquid chromatographic method for chlorpromazine and thirteen metabolites.

A rapid and reliable procedure, based on a C8 bonded phase extraction and reversed-phase isocratic high-performance liquid chromatographic separation with internal standard quantitation, has been developed for the determination of the antipsychotic drug chlorpromazine and thirteen common metabolites. The method allows quantitation of these analytes at the ng/ml concentration range in human plasma. An evaluation of recovery, detection limits, and reproducibility is presented along with application of the method to patient samples.

Biotransformation↗
PubMed1991

Validation of a solid-phase extraction high-performance liquid chromatographic assay for doxazosin.

The determination of doxazosin by high-performance liquid chromatography with fluorescence detection is described. Propanolol was used as the internal standard. Plasma samples were treated with methanol to precipitate the proteins. Doxazosin was isolated with C18 reversed-phase extraction columns. The determination limit is 1 ng/ml of plasma, while the extraction columns can be reused frequently. The method is applied to clinical trial samples.

Adrenergic alpha-Antagonists↗
PubMed1991

Improved high-performance liquid chromatographic method for the routine determination of unconjugated 3-methoxy-4-hydroxyphenylethyleneglycol in human plasma using solid-phase extraction and electrochemical detection.

An improved semi-automated high-performance liquid chromatographic method is described for the routine determination of unconjugated 3-methoxy-4-hydroxyphenylethyleneglycol in plasma. The 3-ethoxy analogue of the compound is used as an internal standard. The method is based on purification of 0.5-ml plasma samples with phenyl-type reversed-phase extraction columns, reversed-phase separation with an acetate-citrate-methanol mobile phase with an octadecyl-bonded column, and dual-electrode coulometric detection with oxidation at +0.44 V and reduction at -0.25 V. The precision and accuracy of the assay are satisfactory: the lower limit of reliable detection corresponds to a plasma concentration of 1.5 nM. The validity of the determination is demonstrated by an 18% mean increase in plasma levels of 3-methoxy-4-hydroxyphenylethyleneglycol during physical exercise (duration 16 min, n = 13) and a 50% mean reduction in plasma levels induced by a single dose of the monoamine oxidase inhibitor, moclobemide (n = 8). The method is suitable for routine use in pharmacological and physiological experiments.

Benzamides↗
PubMed1992

Determination of (+)-5-(2,3-dihydrobenzofuran-7-yl)-3-methyl-8-nitro-2,3,4,5- tetrahydro-1H-3-benzazepin-7-ol (NNC 01-0687), a novel dopamine D-1 receptor antagonist, in plasma by solid-phase extraction and high-performance liquid chromatography.

A fast and reliable method has been established for the determination of the dopamine D-1 receptor antagonist (+)-5-(2,3-dihydrobenzofuran-7-yl)-3-methyl-8-nitro-2,3,4,5-tetrahydro-1 H-3- benzazepin-7-ol (NNC 01-0687) in plasma. A combination of reversed-phase extraction on C18 columns and straight-phase high-performance liquid chromatographic analysis with ultraviolet detection at 287 nm resulted in very clean chromatograms. The limit of quantitation was about 1 ng/ml of plasma. Validation of the method showed good selectivity, linearity, recovery, accuracy and precision. Several modifications of the method were possible with little or no influence on the assay.

Benzazepines↗