Gas-liquid chromatographic determination of chloramphenicol in agricultural crops

A method is presented for the gas-liquid chromatographic determination of chloramphenicol in agricultural crops. Chloramphenicol is extracted with ethyl acetate, cleaned up by silicic acid column chromatography, acetylated with acetic anhydride and pyridine, and then measured by gas-liquid chromatography with electron capture detection. Two stationary phases, DEGS + phosphoric acid and Reoplex 400, were used. The sensitivity was ca 8 ng (40% full scale deflection). The efficicency of the analytical method was evaluated by analyzing crops fortified with chloramphenicol. The average recovery ranged from 72% in unpolished rice to 86% in Chinese radishes.     

Gas-chromatographic determination of chloramphenicol residues in animal material

On the basis of the relevant literature and of their own experimental work, the authors describe extraction, cleaning and derivatization procedures for the determination of chloramphenicol in milk, muscular substance, urine and bile. Chloramphenicol was determined as bis-(trimethylsilyl)-ether using a gas chromatograph fitted with an electron capture detector. To evaluate the analytical techniques, the authors estimated the sensitivity, accuracy and precision for residue amounts of 0.1 and 0.05 mg of chloramphenicol/kg of material under investigation. The limit of detection was 0.02 mg/kg for meat, and 0.01 mg/kg for milk, urine and bile.     

Liquid chromatographic determination of tilmicosin in swine feed at 200-400 mg/kg level: interlaboratory study

An analytical method for the determination of tilmicosin at 200-400 mg/kg, the intended use concentration range, was evaluated in an interlaboratory study involving 5 laboratories, including the sponsor. The interlaboratory study evaluated the intra- and interlaboratory precision and accuracy of a tilmicosin feed method. The method procedure involved extracting tilmicosin from feed by adding 200 mL extractant to 20 g feed and shaking for 1 h. The extract is filtered and analyzed by gradient liquid chromatography which separates tilmicosin from feed matrix in 30 min. Each laboratory assayed 5 replicates of fortified feed at concentrations of 0, 100, 200, 400, and 600 mg/kg. The mean recovery among fortified samples ranged from 81.4 to 98.8%, with a percent coefficient of variation (%CV) ranging from 0.3 to 4.0%. For all blank control feed samples no significant interferences were observed. In addition, each laboratory assayed 5 replicates of medicated feed samples prepared at 2 levels (200 and 400 mg/kg) with either a horizontal or vertical mixer. Along with the medicated feed samples were included 5 replicates of a blank control feed. The identities of the medicated and blank control feed samples were blinded to the analysts. The results for the medicated feed samples ranged from 95.8 to 106% of label claim, with a %CV ranging from 2.1 to 6.7%.     

Gas chromatographic determination of hydrazoic acid

A gas chromatographic procedure was developed for the determination of hydrazoic acid. Two possible columns were evaluated. The limits of detectability were 1.5 ng, or approximately 0.05%, in aqueous solution (w/v) and 2 mg per liter in air.     

Gas chromatographic determination of acenocoumarin in human plasma

A method based on solvent extraction, formation of a fluorinated derivative and quantitation by gas-liquid chromatography with electron-capture detection has been developed for the determination of acenocoumarin in plasma. The specificity and sensitivity of the procedure appear to be satisfactory for drug level measurements in human plasma. Its relative simplicity permits its use in routine analysis.     

Gas chromatographic determination of micro amounts of cyanide residues in wines, distilled liquors, and other alcoholic beverages

A gas chromatographic method for the determination of cyanide residues in alcoholic beverages has been developed from procedures previously reported for application to water samples. Quantitatively isolating HCN from alcoholic beverages presented difficulties not encountered with aqueous solutions, particularly in the presence of S02 in the sample. HCN was liberated from the acidified sample by heating at 70 degrees C, flushed into an NaOH absorber solution, converted to cyanogen bromide (CNBr), extracted into diisopropyl ether, chromatographed on a Porapak Q column, and detected by an electron capture detector. S02 that is present in most wines interfered with the bromination step and caused low recoveries. This interference was eliminated by initially converting any cyanide present in the sample to the stable mercuric cyanide salt and then purging the acidified sample solution of all S02. The Hg(CN)2 present was then dissociated by adding KI and the analysis proceeded as previously described. Mean recoveries of 80-97% were obtained for 2-20 mug cyanide from replicate analyses of spiked samples of distilled liquors free of S02. The relative standard deviations ranged from 6.1 to 11.1%. Mean recoveries of 65 to 91% were obtained in the same range of cyanide from replicate analyses of spiked wine samples known to contain S02, with relative standard deviations ranging from 0.8 to 10.2%. The limit of detection was 0.2 mug HCN.     

A new gas chromatographic determination of ethylenethiourea residues without derivatization

A new gas chromatographic method reliable in the microgram range, was developed to measure ETU residues in various crops. Contrary to previously published procedures, this new method does not require prior derivatization of the ETU. The limit of sensitivity was shown to be 0.01 ppm using the flame photometric detector, FPD (sulfur mode, 394 nm).     

Evaluation of amperometric detector for liquid chromatographic determination of 2-phenylphenol residues in orange rind

A modular component liquid chromatograph has been assembled which has on-stream ultraviolet (UV) and amperometric detectors connected to a dual pen recorder. In this method, the commonly used UV detection technique provides a reference for direct comparisons of results from the amperometric detector. The system has been evaluated and applied to the determination of 2-phenylphenol (2PP) fortified in orange rind. The method is not tedious; before liquid chromatographic analysis, the sample is extracted with methylene chloride and cleaned up on a Florisil column. The method is sensitive to less than 1 ppm 2PP fortified in orange rind; there are no electrically oxidizable interference, from control samples, in the chromatographic region of 2PP. Some background interference does appear from the same samples on the UV chromatogram. Thus, amperometric detection is more specific than UV detection for this application.     

Gas chromatographic determination of pemoline as 5-phenyl-2,4-oxazolidinedione in human urine

A simple gas chromatographic assay of the psychostimulant pemoline in human urine has been developed. Instead of extraction of the drug from urine, it is hydrolysed to 5-phenyl-2,4-oxazolidinedione with 1 N hydrochloric acid. After the extraction, this compound is methylated with diazomethane and determined by gas-liquid chromatography using a nitrogen-selective detector and a solid injection system. The method has been applied in preliminary human pharmacokinetic studies, by measuring the urinary excretion rate of pemoline following oral administration. At present, the screening procedures for doping control do not involve the detection of pemoline, but the method described can easily be incorporated in such procedures.     

Thin-layer chromatographic determination of monensin in feeds: screening method

Monensin is extracted from feed with methanol and purified by solvent-partitioning solid-phase extraction. After solvent reduction, monensin is separated by thin-layer chromatography on silica gel and visualized by color development with vanillin. No false-positive results were obtained in validation studies by submitting or peer laboratories when blank samples were analyzed. Three of 20 samples spiked with 5 ppm monensin were reported as containing no monensin. All samples spiked with 10 ppm monensin were reported positive for monensin.     

Liquid chromatographic determination of ivermectin in feed

An analytical method for determining ivermectin in feed at 0.50-3 ppm is presented. The method is based on liquid chromatographic measurement after sample preparation by adsorption chromatography on alumina and solid-phase extraction. Two complete, final, finished medicated feeds and the corresponding control feeds used in their preparation were analyzed. Recoveries from feeds fortified at 50-150% of the 2 ppm ivermectin use concentration also were determined. Mean recoveries from replicate analyses ranged from 90 to 100%, and coefficients of variation (CVs) were less than 4.5%. No significant interferences were found in control feeds. The pooled distribution of individual analytical results (n = 100) gave a mean recovery of 100%, a recovery range of 90-111%, and an overall CV of 5.5%. Resolution of the total variance into its 2 components gave a within-laboratory CV of 4.1% and a between-laboratory CV of 3.4%. There was no significant difference in recoveries among laboratories, days, concentrations, and feed base or between fortified and medicated feeds (P > 0.2).     

Gas chromatographic determination of Ostwald solubility coefficients for cyclopropane, halothane and trichloroethene (trichloroethylene)

Gas chromatographic methods using solvent extraction for the analysis of cyclopropane and and trichloroethene (trichloroethylene) are described and evaluated; cyclopropane was extracted into carbon tetrachloride and trichloroethene into carbon disulphide, using chloroform and toluene respectively as the internal standards. Ostwald solubility coefficients were measured for cyclopropane, halothane and trichloroethene in Krebs solution: at 310 K the respective values +/- SEM of the Ostwald coefficients are 0.181 +/- 0.009, 0.78 +/- 0.02 and 1.54 +/- 0.02; over the temperature range 295-310 K the respective temperature coefficients of solubility are -2.27, -4.18 and -3.81 in units of per cent/K at 310 K.