Gas chromatographic method for the simultaneous determination of dopamine and norepinephrine metabolites

A new gas chromatographic method, using only flame ionization detection which can determine nanogram quantities of homovanillic acid, 3,4-dihydroxyphenylacetic acid, 3-methoxy-4-hydroxyphenylethyleneglycol and 3,4-dihydroxyphenylethyleneglycol in the same reaction, is described. These compounds are treated with diazoethane and n-butylboronic acid. Homovanillic acid and 3,4-dihydroxyphenylacetic acid are converted to their ethyl esters while 3-methoxy-4-hydroxyphenylethyleneglycol and 3,4-dihydroxyphenylethyleneglycol from cyclic boronates and are thus assayed. This method is quantitative, highly specific and sensitive. It has been applied to the analysis of these compounds in urine.     

Improved high-performance liquid chromatographic method for the determination of polycyclic aromatic hydrocarbon metabolites in human urine

A reversed-phase HPLC method with fluorescence detection was evaluated for utility in determination of urinary metabolites of polycyclic aromatic hydrocarbons as biomarkers of environmental exposure. The method, which was developed for use in studies of high-level occupational exposure, was found to be unreliable for relatively low-level environmental exposures. The method was modified to include quantitation by standard addition in order to compensate for matrix effects at levels as low as 0.1 ng/ml. The standard addition modification increased both qualitative and quantitative performance, with recovery of 1-hydroxypyrene spikes improved from 164% to 114% at 0.36 ng/ml. The modified method was successfully applied in an environmental exposure study.     

Gas chromatographic determination of amino acid enantiomers in bottled and aged wines

Free l- and d-amino acids were determined by chiral GC-MS in 26 wines, comprising white wines, red wines, ice wines and sparkling wines. The aim of the work was to investigate whether quantities and pattern of d-amino acids, in particular d-proline, correlate with the storage time of bottled wines. The relative quantities with respect to the corresponding l-enantiomer ranged in white wines from 0.4 to 3.9% d-Ala, 0.9–8.3% d-Asx, and 0.5–8.9% d-Glx, in red wines from 2.9 to 10.6% d-Ala, 2.2–10.9% d-Asx, and 3.9–7.4% d-Glx, and in sparkling wines from 2.2 to 9.8% d-Ala, 2.1–4.4% d-Asx and 1.3–6.1% d-Glx. Low relative quantities of 0.3–0.7% d-Pro were detected in three white wines stored for more than 20 years and did not exceed 0.2% d-Pro in two red wines stored for 10 and 20 years, respectively. An ice wine stored for 24 years contained 0.9% d-Pro, 6.4% d-Glx, 3.0% d-Asp and 1.5% d-Ala. The data confirm the presence of d-amino acids in wines. They do not provide evidence for a correlation between the storage time of bottled wines and quantities of d-amino acids.     

Gas chromatographic determination of amino acid configuration in the optically active stationary phase

The synthesis and physico-chemical properties of a novel optically active stationary phase--N-stearoyl-L-valyl-t-butylamide (I) applied for GLC separation of enantiomeric alpha-amino acids are described. The optical purity of the compound (I) is not less than 85%. The efficiency of the phase is shown on analyses of the configuration of amino acids in peptidolipids and glycopeptidolipids produced by the paraffin-oxidizing bacterium Mycobacterium paraffinicum.     

Gas chromatographic determination of thymol.

Thymol in biological samples is analyzed by gas chromatography utilizing a 5% OV-25 column, a flame ionization detector, and eugenol as an internal standard. Samples are extracted with diethyl ether and analyzed without derivatization. The lower limit of detection of thymol in a sample is about 0.01 μg and quantitation is satisfactory in plasma at $\text{0.05 μ}\text{g}\text{2}\text{ml}$. Data was recorded digitally on magnetic tape and calculated off-line at a central facility.     

Gas chromatographic determination of glutamine in the presence of glutamic acid in biological fluids

The gas chromatographic determination of glutamine and glutamic acid in biological samples has so far presented considerable difficulties due to rapid conversion of glutamine to glutamic acid during derivatization. Quantitation of glutamine can be based on an intermediate in the above reaction, i.e. pyrrolidone carboxylic acid. However, the percentage formed is strongly dependent on reaction conditions, rendering quantitation unreliable. To overcome this problem d-glutamine, the optical isomer to the natural l-glutamine, is added as internal standard. The enantiomers are chemically identical and form the cyclic derivative to the same extent. The enantiomers of pyrrolidone carboxylic acid ester can easily be separated on a capillary coated with the chiral stationary phase Chirasil-Val. No extra derivatization step is required and quantitation is based merely on the ratio of the peak areas of both enantiomers.     

Gas chromatographic determination of low concentrations of benzoic acid in human plasma and urine

A method for the determination of benzoic acid down to concentrations of 10 ng/ml in plasma or urine is described. After addition of an internal standard, benzoic acid is extracted at acid pH into diethyl ether. Both compounds are derivatized with pentafluorobenzyl bromide. The derivatives are determined by gas chromatography using a ⁴³Ni electron-capture detector. Hippuric acid is hydrolysed in plasma and urine and total benzoic acid is determined by the same technique.     

Gas chromatographic determination of meprobamate in human plasma

A simplified and rapid gas chromatographic method has been developed for the determination of meprobamate in human plasma. The procedure includes a single-step extraction of alkalinized sample with chloroform, and chromatography on a non-polar fused-silica capillary column with flame ionization detection. The method is accurate (97.7 ± 5.7% at 20 mg/l) and precise (maximum coefficient of variation of 9.5%). It provides an alternative to existing methods and is particularly suitable for toxicological studies.     

Gas chromatographic determination of sodium dodecyl sulfate

A gas chromatographic method has been developed for the determination of sodium dodecyl sulfate. The method is sensitive, reasonably accurate, and uninfluenced by the presence of protein. The method depends upon the formation of 1-dodecanol and inorganic sulfate by acidic hydrolysis of sodium dodecyl sulfate (4 n HCl, 2 hr, 100°C). The ether extracted 1-dodecanol is analyzed by standard gas chromatographic techniques.     

A chromatographic determination of gibberellic acid

1. (1)
   Гибберелловую кислоту можно определить хроматографически в ферментационной Зидкости, в препаратах гиббереллина и в различных стадиях экстракции при помощи буферной бумаги и n-амилацетата. Синие пятна, получаемые после применения реагента Folin-Ciocîlteu смывают и окраску определяют фотометрически.     
   
   

Liquid chromatographic determination of mycophenolic acid and its metabolites in human kidney transplant plasma: pharmacokinetic application

BACKGROUND AND OBJECTIVE: Difference in the hydrophilic properties of mycophenolic acid metabolites makes it technically difficult to simultaneously determine their plasma levels in one analytical run. Therapeutic drug monitoring (TDM) for MPA ensures adequate MPA exposure levels to both prevent rejection and avoid related toxicity. One measure limitation for TDM for MPA is the availability of simple, rapid and reproducible method for determination of MPA derivatives. METHOD: Herein we report a single method to measure MPA and its metabolites using a gradient elution system in less than 10 min. We further tested applicability of our method in both stable and unstable renal transplant recipients with a wide range of levels. RESULTS: Intra- and inter-day imprecision were less than 8% and 10%, respectively. Accuracy of the estimated concentrations ranges from 90% to 108%. CONCLUSION: Collectively these data show that the new method is reasonably accurate and precise for the simultaneous determination of MPA and its metabolites in human plasma.