Determination of amphetamine by Schiff base formation and quantitative gas-liquid chromatography.

A procedure was developed to determine amphetamine salts in solid dosage forms. Amphetamine was extracted from the solid matrix with dilute hydrochloric acid and reacted with cyclohexanone in a strongly basic aqueous methanolic solution. The Schiff base reaction product was extracted with hexane for gas chromatographic determination. Reaction time and optimum conditions were studied. Phenethylamine, similarly treated, was used as an internal standard. Results compared favorably with those obtained by using USP methods.     

Determination of zearalenone in cornflakes and other corn-based foods by thin layer chromatography, high pressure liquid chromatography, and gas-liquid chromatography/high resolution mass spectrometry

A simple cleanup procedure based on pH adjustments was used to obtain extracts of corn foods. The method gave good recoveries of zearalenone determined by thin layer chromatography (TLC) and high pressure liquid chromatography (HPLC). As little as 5 ng zearalenone was detected by TLC, using Fast Violet B Salt as the spray reagent; the lower limit of detection in cornflakes was about 20 microgram/kg. With HPLC on Spherisorb silica (5 micrometer) and detection by fluorescence at an excitation maximum of 310 nm as little as 5 microgram zearalenone/kg cornflakes could be determined. While the TLC method was also applicable to corn chips, cornmeal, popcorn, and frozen corn, an interference was observed in HPLC of the latter 3 products. This interference was separated from zearalenone by adding a second HPLC analytical column (Spherisorb ODS). Gas-liquid chromatography coupled with mass spectrometric single ion monitoring at high resolution, although of limited availability, was shown to be the most sensitive and selective method for determining zearalenone in corn foods. The natural occurrence of zearalenone in a sample of cornflakes (13-20 microgram/kg) was demonstrated by all 3 detection procedures.     

Determination of total sulfur in soils and plant materials by ion chromatography

Abstract

An accurate and precise ion Chromatographie (IC) method is described for determination of total S in soils and plant materials. It involves ignition of a mixture of soil and NaHCO₃or plant material and NaHCO₃containing Ag₂O at 550°C for 3 h. The residue is dissolved in 1MHOAc, diluted with deionized water, filtered, and analyzed for S0^2‐ ₄by a Dionex model 2002i ion Chromatograph. Results by the IC method of seven Iowa soils, three Chilean soils, and 10 plant materials agreed closely with those obtained by the methylene blue method after alkaline oxidation with NaOBr. In general, the IC method was more precise than the methylene blue method. The method is simple and requires a minimum of analytical skill. A single operator can analyze 30–40 soil or plant samples in a normal working day.     

Determination of borate in extracts of gypsiferous soils by single column ion chromatography

Abstract

A high performance liquid chromatography apparatus with a resin based anion exchange column and a conductivity detector were used to develop a method for borate separation and quantification in extracts of gypsiferous soils. An eluant containing 5 mMNaOH and 0.5 mMNa‐benzoate was found to produce satisfactory chromato‐grams. Calibration curves were linear in the range l to 7 mg B/L. The recovery of ? in spiked samples had a mean and coefficient of variation of 99.6 and 2.2 percent, respectively. The presence of divalent cations caused baseline instability that was remedied by exchange with H⁺using Dowex 50–8X. The presence of sulfate extended analysis time and was removed by precipitation with BaCl₂. Coloration by organic matter does not interfere with ? determination by this method, but individual simple organic acids may mask the borate peak     

Extraction and cleanup of organochlorine, organophosphate, organonitrogen, and hydrocarbon pesticides in produce for determination by gas-liquid chromatography.

A rapid, multiresidue procedure utilizing the minimal cleanup necessary for gas-liquid chromatographic (GLC) analysis is presented. The samples are extraced with acetone and partitioned with methylene chloride-petroleum either to remove water. The organophosphorus and organonitrogen compounds are then quantitated by GLC, using a KCl thermionic detector. A Florisil cleanup of the extract is performed prior to the determination of organochlorine compounds by a GLC electron capture detector. Carbon-hydrogen compounds such as biphenyl and o-phenylphenol undergo the Florisil cleanup and may also be quantitated by GLC. Quantitative recoveries for 15 organophosphorus, 9 organochlorine, 5 organonitrogen, and 2 hydrocarbon pesticides show the range in polarities of pesticides recovered, from Monitor to biphenyl. The method is simple and fast with a great potential for the analysis of many more compounds.     

Determination of gossypol enantiomer ratio in cotton plants by chiral higher-performance liquid chromatography

A celulose tris(3,5-dimethylphenylcarbamate) coated onto APS silica (Nucleosil, particle size, 7 microm; pore size, 500 A) was used under a reversed-phase condition to measure the enantiomeric ratios of gossypol enantiomers in cottonseeds, flowers, and roots in a number of cultivars samples of different Gossipium species. While unidimensional chromatography was used for measuring the enantiomeric ratio of all the samples of G. hirsutum, G. mustelinum, and in the seeds of G. barbadense, multidimensional chromatography was necessary for the analysis of samples of roots and flowers of G. barbadense. In the latter case, an ODS Hypersil column was used in the first dimension for sample clean up, and the enantiomers were resolved on the second dimension by the chiral column. As expected, all the seed samples of G. hirsutum and G. mustelinum showed the (P)-(+)-enantiomer in excess, whereas the seeds of G. barbadense showed the (M)-(-)-enantiomer. However, (P)-(+)-gossypol was found in enantiomeric excess in three samples examined of roots and in one of flower of G. barbadense. These results are discussed in this paper.