Liquid-chromatographic determination of 5-S-L-cysteinyl-L-dopa with electrochemical detection in urine prepurified with a phenylboronate affinity gel.

1983 ◽  
Vol 29 (12) ◽  
pp. 2031-2034 ◽  
Author(s):  
B Kågedal ◽  
A Pettersson

Abstract A phenylboronate affinity gel has been investigated for use in the prepurification of urine before "high-performance" liquid chromatography and electrochemical determination of 5-S-L-cysteinyl-L-dopa. At pH 5.6 this naturally occurring 5-S-cysteinyldopa was adsorbed on a phenylboronate column and was quantitatively eluted with trichloroacetate, pH 3.0. This pretreatment of urine before "high-performance" liquid chromatography produced satisfactory chromatographic separations, and the results were further improved when the purification procedure also included treatment on a cation exchanger. By using 5-S-D-cysteinyl-L-dopa--a diastereomer to 5-S-L-cysteinyl-L-dopa--as an internal standard, we have developed a practical routine method for the quantitative determination of urinary 5-S-L-cysteinyl-L-dopa. The precision (CV = 2.4%) and analytical recovery (96.9%, SD 5.3%) were satisfactory and the results obtained correlated well with a previously described method.

1986 ◽  
Vol 32 (6) ◽  
pp. 1002-1004 ◽  
Author(s):  
H Hughes ◽  
L Hagen ◽  
R A Sutton

Abstract In this method for 4-hydroxyproline in urine, hydroxyproline is derivatized with 4-chloro-7-nitrobenzofurazan, with subsequent estimation by reversed-phase "high-performance" liquid chromatography. The ranges for excretion of free and total hydroxyproline while the subjects were ingesting unrestricted diets were 2-29 and 122-374 mumol/24 h (n = 21), respectively, with no significant sex-related difference. A comparison with results by colorimetry indicated no significant differences: mean (n = 18) concentrations (mumol/L) of hydroxyproline in urine were 180 (SD 149) by the present method, 163 (SD 166) by colorimetry. For protein hydrolysate the respective values were 5.9 (SD 2.7) and 6.7 (SD 2.9).


1982 ◽  
Vol 65 (6) ◽  
pp. 1302-1304
Author(s):  
Yoshimi Kitada ◽  
Michiko Sasaki ◽  
Kaoru Tanigawa

Abstract A simple, rapid, efficient method has been developed for determining thiabendazole, o-phenylphenol, and diphenyl in citrus fruits by using high performance liquid chromatography, with fluorescence or ultraviolet detection. The compounds are extracted with ethyl acetate and separated from soluble fruit components on a LiChrosorb RP-8 column. Recovery of these compounds added to citrus fruits at 5 or 50 ppm levels was >93%; the limit of detection for the compounds is 1 ppm.


1979 ◽  
Vol 62 (6) ◽  
pp. 1338-1341
Author(s):  
Elizabeth Cox

Abstract High performance liquid chromatography was used to determine quinizarin, p-toluidine, and D&C Violet No. 2 in D&C Green No. 6. Recoveries averaging 102, 105, and 104% were obtained for quinizarin, p-toluidine, and D&C Violet No. 2, respectively. Multiple runs on one sample of D&C Green No. 6 indicated variability in the amount of p-toluidine found.


2003 ◽  
Vol 68 (11) ◽  
pp. 883-892 ◽  
Author(s):  
Dragica Zendelovska ◽  
Trajce Stafilov

A rapid, specific and sensitive high-performance liquid chromatographic method for the determination of famotidine in human plasma has been developed. Famotidine and the internal standard were chromatographically separated from plasma components using a Lichrocart Lichrospher 60 RP select B cartridge for solid-phase separation with a mobile phase composed of 0.1 % (v/v) triethylamine in water (pH 3) and acetonitrile (92:8, v/v). UV detection was set at 270 nm. The calibration curve was linear in the concentration range of 10.0 ? 350.0 ng mL-1. The method was implemented to monitor the famotidine levels in patient samples.


1984 ◽  
Vol 30 (7) ◽  
pp. 1228-1230 ◽  
Author(s):  
A K Dhar ◽  
H Kutt

Abstract This method for determination of haloperidol in plasma is based on "high-performance" isocratic liquid chromatography with the use of a C8 bonded reversed-phase column at room temperature. Haloperidol and the internal standard (chloro-substituted analog) are extracted from alkalinized plasma into isoamyl alcohol/heptane (1.5/98.5 by vol) and back-extracted into dilute H2SO4. The aqueous phase is directly injected onto the column. The mobile phase is a 30/45/25 (by vol) mixture of phosphate buffer (16.5 mmol/L, pH 7.0), acetonitrile, and methanol. Unlike other liquid-chromatographic procedures for haloperidol, commonly used psychotropic drugs do not interfere. Analysis can be completed within an hour. The procedure is extremely sensitive (1.0 microgram/L) and is well reproducible (CV 5.6% for a 2.5 micrograms/L concentration in plasma).


1982 ◽  
Vol 65 (3) ◽  
pp. 753-756
Author(s):  
Walter F Schmidt

Abstract A high performance liquid chromatographic procedure has been developed for the assay of phenprocoumon in tablets. In comparison to the present official USP assay procedure, it is equivalent in precision and accuracy and is faster and more specific. A mobile phase consisting of a 1% solution of acetic acid in acetonitrile-water (4 + 3) separates phenprocoumon from warfarin internal standard on a 6 μm octadecylsilane (ODS) column with UV detection at 311 nm. The method enables the concurrent determination of phenprocoumon and possible contaminants such as salicylic acid.


1976 ◽  
Vol 59 (3) ◽  
pp. 675-677
Author(s):  
Randolph H Dyer ◽  
Glenn E Martin ◽  
Peter C Buscemi

Abstract Wine samples containing β-asarone (cis-2,4,5-trimethoxy-1-propenylbenzene) are distilled; β-asarone is extracted by hexane and then quantitatively determined by gas-liquid chromatography (GLC), using ethyl palmitate as the internal standard. The GLC procedure is rapid and yields precise and accurate results. Mass spectrometery confirmed the identity of the GLC peak as β-asarone. The ultraviolet spectra of β-asarone and its isomer were also determined.


1986 ◽  
Vol 32 (5) ◽  
pp. 816-818 ◽  
Author(s):  
E Schoenau ◽  
K H Herzog ◽  
H J Boehles

Abstract We describe a new method for separating alkaline phosphatase (AP) isoenzymes by means of "high-performance" liquid chromatography. Isoenzymes are eluted from the column (Mono Q HR 5/5, a strong anion-exchanger) with a stepwise gradient of LiCl. The isoenzymes originating from small intestine, bone, liver, and bile were identified by use of tissue homogenates, pathological sera, and heat inactivation.


1978 ◽  
Vol 61 (1) ◽  
pp. 68-71
Author(s):  
Dorothy K Wyatt ◽  
Lee T Grady

Abstract Gas-liquid chromatography (GLC) coupled with column chromatography was used to accurately determine as little as 25 ppm p-chloroacetanilide in acetaminophen. p-Chloroacetanilide was eluted from a pH 8 phosphate-buffered diatomite partition column by using purified tetrachloroethylene (acetaminophen was retained). This solution was concentrated, internal standard (docosane) was added, and p-chloroacetanilide was determined by using a 0.9 m × 2 mm glass column packed with 3% Poly A 103 on Supelcoport and a flame ionization detector with electronic integration. Standard curves were linear for 10–100 ppm p-chloroacetanilide. Various chromatographic materials were investigated for optimal retention characteristics. High pressure liquid chromatography (HPLC) was also evaluated as an alternative; however, lack of reproducibility of the HPLC column favored the GLC procedure.


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