Mannitol estimation in biological fluids by gas-liquid chromatography of trimethylsilyl derivatives.

1980 ◽  
Vol 26 (3) ◽  
pp. 441-443 ◽  
Author(s):  
M F Laker ◽  
J N Mount

Abstract We describe a procedure for estimating mannitol concentrations in biological fluids. Samples are mixed with internal standard solution (alpha-methylglucose), deproteinized if necessary, desalted, and dried. Specimens are then derivatized by adding pyridine/bis(trimethylsilyl)acetamide/trimethylchlorosilane and heating at 60 degrees C for 30 min. Samples are chromatographed on a 275-cm column of 10% OV-17, operated at 190 degrees C, and quantitated by peak-height measurement. The technique is linear, accurate, precise, sensitive, and free from interference. It has been used to measure mannitol in plasma, urine, and bile.

1980 ◽  
Vol 26 (3) ◽  
pp. 441-443 ◽  
Author(s):  
M F Laker ◽  
J N Mount

Abstract We describe a procedure for estimating mannitol concentrations in biological fluids. Samples are mixed with internal standard solution (alpha-methylglucose), deproteinized if necessary, desalted, and dried. Specimens are then derivatized by adding pyridine/bis(trimethylsilyl)acetamide/trimethylchlorosilane and heating at 60 degrees C for 30 min. Samples are chromatographed on a 275-cm column of 10% OV-17, operated at 190 degrees C, and quantitated by peak-height measurement. The technique is linear, accurate, precise, sensitive, and free from interference. It has been used to measure mannitol in plasma, urine, and bile.


1968 ◽  
Vol 51 (5) ◽  
pp. 959-963
Author(s):  
S W Gunner ◽  
B Hand ◽  
M Sahasrabudhe

Abstract The qualitative and quantitative analysis of maltol and ethyl maltol in apple juice is described. The compounds were extracted with ethyl acetate and, after the addition of 2,6-dimethoxyphenol as internal standard, they were analyzed by gas-liquid chromatography as such or as their trimethylsilyl derivatives. Recovery of maltol and ethyl maltol was dependent on the method of isolation and ranged from 92 to 97.5% in the method of choice


1984 ◽  
Vol 219 (3) ◽  
pp. 883-889 ◽  
Author(s):  
A Gorchein

A derivative of delta-aminolaevulinic acid (AmLev), 2-methyl-3-acetyl-4-(3-propionic acid pentafluorobenzyl ester)pyrrole, with favourable properties for g.l.c. with electron-capture detection, was synthesized. Less than 1 pg could be detected on the column. 6-Amino-5-oxohexanoic acid formed the analogous derivative under similar conditions and was used as the internal standard in the development of a highly sensitive and specific assay for AmLev. The method has been applied to peripheral-venous and umbilical-cord plasma and to cerebrospinal fluid of normal and porphyric subjects.


1990 ◽  
Vol 70 (4) ◽  
pp. 1097-1103 ◽  
Author(s):  
G. W. DUYNISVELD ◽  
B. A. SLOMINSKI ◽  
K. M. WITTENBERG ◽  
L. D. CAMPBELL

A technique was developed for the quantification of gramine, hordenine and 5-methoxy-N,N-dimethyl tryptamine (5MeO-DMT) in reed canarygrass (RCG) using gas–liquid chromatography. One gram of freeze-dried, ground RCG sample was extracted with methanol containing 1% ammonium hydroxide. Following solvent evaporation, the residue was extracted with dilute hydrochloric acid (0.01 N). The pH of the extract was then raised and stabilized by adding 0.5 M sodium tetraborate-boric acid buffer pH 9. The internal standard solution (0.25 mg mL−1) n-nonadecane was added and the extract was purified by partitioning with chloroform. The chloroform was then evaporated and the alkaloids were derivatized with bis(trimethylsilyl)-trifluoroacetamide and effectively separated on a gas chromatographic column packed with 2% OV-7 on Chromosorb W. Derivatization was effective at 100 °C (20 min). Extraction of the sample with methanol was maximal at 30-minute extraction time and the recovery of all the alkaloids studied was shown to average 90%. Development of this procedure provides a means to measure RCG gramine, hordenine and 5MeO-DMT concentrations in the presence or absence of tryptamines or β-carbolines. Initial growth and regrowth of five cultivars of RCG from two locations were evaluated for gramine, hordenine and 5MeO-DMT content using this technique. No differences were detected in hordenine content. Gramine content was higher (P < 0.05) in Rival than Venture, with Castor, Palaton and Vantage being intermediate. None of the cultivars contained detectable levels of 5MeO-DMT. There were no differences (P > 0.05) in hordenine content between initial growth and regrowth; however, gramine content of regrowth was higher (P < 0.05) than initial growth.Key words: Gramine, hordenine, 5-methoxy-N,N-dimethyl tryptamine, reed canarygrass, Phalaris arundinaceae L.


1979 ◽  
Vol 57 (5) ◽  
pp. 534-538 ◽  
Author(s):  
Joe E. Webber ◽  
Murray L. Laver ◽  
Joe B. Zaerr ◽  
Denis P. Lavender

The occurrence of abscisic acid (ABA) in the dormant shoots of Douglas-fir (Pseudotsuga menziesii (Mirb.) Franco) was confirmed by bioassay, thin-layer chromatography, gas–liquid chromatography, and gas–liquid chromatography – mass spectrometry. Seasonal variation of ABA in the buds, leaves, and stems was then determined using 2-trans-ABA as an internal standard. Concentrations of ABA were highest in the autumn for buds (2.1 μg/g) and needles (0.79 μg/g) and highest in January for stems (0.34 μg/g). The lowest concentrations for all tissues were in February and March, before bud burst. Close correlation of levels of ABA with previously measured physiological evidence of growth and metabolic activity suggests a possible role in the dormancy cycle of Douglas-fir.


1971 ◽  
Vol 51 (3) ◽  
pp. 447-454 ◽  
Author(s):  
W. COOPER ◽  
M. G. COYLE ◽  
J. A. MILLS

SUMMARY A method is described for estimating oestriol in 2–10 ml samples of human pregnancy peripheral plasma. It incorporates acid hydrolysis, chemical purification, methylation, chromatography on alumina columns, formation of a derivative and quantitative determination by gas chromatography. A radioactive internal standard was added to correct for procedural losses. Plasma oestriol determinations in five normal patients throughout pregnancy and delivery are reported.


1977 ◽  
Vol 23 (7) ◽  
pp. 1306-1309 ◽  
Author(s):  
R H Smith ◽  
J A MacDonald ◽  
D S Thompson ◽  
W E Flacke

Abstract We describe an isothermal gas-liquid chromatographic procedure developed for measuring thiamylal and thiopental in plasma. The unchanged drug is extracted into ethyl acetate from acidified plasma, together with an internal standard. The solvent is removed, the residue methylated, aliquots, diluted with benzene, are injected into a 183-cm gas-liquid chromatographic column containing 3% OV-17. Sensitivity of detection is in the nanogram to picogram range.


1978 ◽  
Vol 24 (10) ◽  
pp. 1821-1823 ◽  
Author(s):  
A J Fellenberg ◽  
A C Pollard

Abstract A gas-liquid chromatographic procedure for the microdetermination of ethosuximide is described. Ethosuximide is extracted from acidified plasma or serum into chloroform containing an internal standard alpha,alpha-dimethyl-beta-methyl succinimide. Part of the initial chloroform extract is gently evaporated, the residue redissolved in n-heptane at 60 degrees C, and an aliquot analyzed by gas-liquid chromatography. The procedure is rapid, reliable, sensitive, and specific. It requires a 25--50 microliter sample for a single estimation, has a detection threshold of less than 10 micromol/liter, and is suitable for routine clinical use.


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