Improved liquid-chromatographic method for determination of serum cortisol.

1979 ◽  
Vol 25 (7) ◽  
pp. 1293-1296 ◽  
Author(s):  
P M Kabra ◽  
L L Tsai ◽  
L J Marton
Keyword(s):  
Limit Of Detection ◽  
Internal Standard ◽  
Serum Cortisol ◽  
Peak Height ◽  
Reversed Phase ◽  
Column Temperature ◽  
Coefficients Of Variation ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic

Abstract We describe a specific and precise method for measuring concentrations of cortisol in serum or plasma by liquid chromatography. Cortisol, together with an internal standard, equilenin, is extracted from 1 mL of serum or plasma and analyzed isocratically on a reversed-phase column with a mobile phase of acetonitrile/phosphate buffer (30/70, by vol.), at a flow rate of 2.0 mL/min. The eluted cortisol is detected by its absorption at 254 nm and quantitated by peak height measurements. Each analysis requires no longer than 15 min at the optimum column temperature of 50 degrees C. The lower limit of detection for cortisol is about 2 ng/sample for a standard solution; sensitivity is routinely 5 micrograms/L of serum. Analytical recoveries exceeded 95%, with good day-to-day precision (coefficients of variation between 4 and 7%). Of more than 50 drugs and steroids tested for possible interference, only the steroids cortisone, prednisone, and prednisolone may interfere with the analysis of cortisol.

Simultaneous liquid-chromatographic determination of 12 common sedatives and hypnotics in serum.

1978 ◽  
Vol 24 (4) ◽  
pp. 657-662 ◽  
Author(s):  
P M Kabra ◽  
H Y Koo ◽  
L J Marton
Keyword(s):  
Serum Proteins ◽  
Limit Of Detection ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Reversed Phase ◽  
Acetonitrile Solution ◽  
Column Temperature ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract We present a method for simultaneously determining 12 hypnotics and sedatives (primidone, methyprylon, phenobarbital, butabarbital, butalbital, ethchlorvynol, pentobarbital, amobarbital, phenytoin, glutethimide, secobarbital and methaqualone) in 200 microliter of serum. Serum proteins are precipitated with an acetonitrile solution containing 5-(4-methylphenyl)-5-phenylhydantoin, the internal standard. The drugs are eluted from a reversed-phase column with a mobile phase consisting of an acetonitrile/phosphate buffer, at a flow rate of 3.0 ml/min. The eluted drugs are detected by their absorption at 195 nm; their quantities are estimated from their peak heights. Each analysis requires no longer than 30 min at the optimum column temperature of 50 degrees C. The lower limit of detection for all of these drugs is less than 10 ng/sample for drug standard. A sensitivity of 1.0 mg/liter of serum is attained routinely for each of the drugs. Analytical recoveries for the 12 drugs varied from 94 to 112%, with good day-to-day precision (CV between 3.8 and 10.4%). Of more than 35 drugs tested for possible interference, only ethotoin interferes with the analysis of phenobarbital.

Improved liquid-chromatographic determination of mexiletine, an antiarrhythmic drug, in plasma.

1984 ◽  
Vol 30 (2) ◽  
pp. 319-322 ◽  
Author(s):  
W Mastropaolo ◽  
D R Holmes ◽  
M J Osborn ◽  
J Rooke ◽  
T P Moyer
Keyword(s):  
Methylene Chloride ◽  
Limit Of Detection ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Peak Height ◽  
Reversed Phase ◽  
Internal Standard Peak ◽  
Chromatographic Procedure ◽  
Liquid Chromatographic

Abstract In this improved reversed-phase liquid-chromatographic procedure for determination of mexiletine in plasma, mexiletine and an internal standard, chlorodisopyramide, are extracted with methylene chloride from 0.5 mL of serum or plasma; the extract is then concentrated and injected onto a C18 chromatographic column. Mexiletine in the column effluent is detected by monitoring absorbance at 210 nm. It is quantified by use of mexiletine-internal standard peak-height ratios. The relation between this ratio and mexiletine concentration is linear from 0.1 to 5.0 mg/L. The lower limit of detection is about 50 micrograms/L. At a mexiletine concentration of 2.0 mg/L in serum, intrarun precision (CV) is 2.9% and inter-run precision is 5.9%; at 0.5 mg/L, these CVs are 5.7% and 9.6%, respectively. Analytical recovery of added mexiletine in serum is 68-88%. Therapeutic concentrations of some commonly administered drugs in patients' specimens did not interfere. In serum from 38 patients receiving mexiletine for cardiac arrhythmia, concentrations measured by this method correlated with therapeutic efficacy.

Liquid-chromatographic determination of tobramycin in serum with spectrophotometric detection.

1983 ◽  
Vol 29 (4) ◽  
pp. 672-674 ◽  
Author(s):  
P M Kabra ◽  
P K Bhatnagar ◽  
M A Nelson ◽  
J H Wall ◽  
L J Marton
Keyword(s):  
Limit Of Detection ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Reversed Phase ◽  
Water Soluble ◽  
Trinitrobenzenesulfonic Acid ◽  
Column Temperature ◽  
Derivatizing Agent ◽  
Liquid Chromatographic

Abstract We describe a simple, precise, accurate, and specific liquid-chromatographic procedure for determination of tobramycin in 50 microL of serum. Tobramycin and the internal standard (sisomicin) are quantitatively converted into their trinitrophenyl derivatives by reaction with a water-soluble derivatizing agent (2,4,6-trinitrobenzenesulfonic acid) at 70 degrees C for 30 min. The derivatives are extracted from the crude reaction mixture by using a reversed-phase Bond-Elut C18 column, and separated on a reversed-phase octyl column with a mobile phase consisting of an acetonitrile/phosphate buffer (70/30 by vol) at a flow rate of 3.0 mL/min. The eluted compounds are detected at 340 nm, and quantified from their peak areas. Chromatography is complete in less than 4.5 min at the optimum column temperature of 50 degrees C. The lower limit of detection for tobramycin is less than 0.2 mg/L. Analytical recoveries for tobramycin varied from 94 to 99%, linearity extended to 25 mg/L, and day-to-day precision (CV) was between 4.6 and 5.1%. Numerous drugs and antibiotics tested do not interfere. Results correlate well (r greater than 0.95) with those by radioimmunoassay and EMIT.

Gas-Liquid Chromatographic Determination of T-2 Toxin in Plasma

1983 ◽  
Vol 66 (4) ◽  
pp. 909-912 ◽  
Author(s):  
Steven P Swanson ◽  
Venkatachalam Ramaswamy ◽  
Val R Beasley ◽  
William B Buck ◽  
Harold H Burmeister
Keyword(s):  
Chromatographic Method ◽  
Limit Of Detection ◽  
Internal Standard ◽  
Aqueous Sodium Hydroxide ◽  
Chromatographic Determination ◽  
Florisil Column ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract The gas-liquid chromatographic method for the determination of T-2 toxin in plasma is described. The toxin is extracted with benzene, washed with aqueous sodium hydroxide, and chromatographed on a small Florisil column; the heptafluorobutyryl derivative is prepared by reaction with heptafluorobutyrylimidazole. The T-2 HFB derivative is chromatographed onOV-1 at 230°C and measured with an electron capture detector. Iso-T-2, an isomer of T-2 toxin, is added to samples as an internal standard before extraction. Recoveries averaged 98.0 ± 5.5% at levels ranging from 50 to 1000 ng/m L. The limit of detection is 25 ng/mL.

Determination of Acesulfam-K in Foods

1993 ◽  
Vol 76 (2) ◽  
pp. 268-274 ◽  
Author(s):  
Jacques Prodolliet ◽  
Milene Bruelhart
Keyword(s):  
Fruit Juice ◽  
Soft Drink ◽  
Food Additives ◽  
Reversed Phase ◽  
Uv Absorbance ◽  
Phase Detection ◽  
Coefficients Of Variation ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic

Abstract A liquid chromatographic method was evaluated for the determination of the intense sweetener acesulfam-K in tabletop sweetener, candy, soft drink, fruit juice, fruit nectar, yogurt, cream, custard, chocolate, and biscuit commercial preparations. Samples are extracted or simply diluted with water and filtered. Complex matrixes need a clarification step with Carrez solutions. An aliquot of the extract is analyzed on a reversed-phase μBondapak C18 column using 0.0125M KH2PO4 (pH 3.5)-acetonitrile (90 + 10) as mobile phase. Detection is performed by UV absorbance at 220 nm. Recoveries ranged from 95.2 to 106.8%. With one exception, all analyzed values were within ±15% of the declared levels. The repeatabilities and the repeatability coefficients of variation were, respectively, 0.37 mg/100 g and 0.98% for products containing less than 40 mg/100 g acesulfam-K and 2.43 mg/100 g and 1.29% for other products. The same procedure also allowed detection of many food additives or natural constituents, such as other intense sweeteners, organic acids, and alkaloids, in a single run without interfering with acesulfam-K. The method is simple, rapid, precise, and sensitive; therefore, it is suitable for routine analyses.

Liquid Chromatographic Determination of Triadimefon in Technical and Formulated Products: Collaborative Study

1985 ◽  
Vol 68 (3) ◽  
pp. 586-589
Author(s):  
Stephen C Slahck
Keyword(s):  
Collaborative Study ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Normal Phase ◽  
Coefficients Of Variation ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
Technical Products

Abstract A liquid chromatographic method for the determination of triadimefon (Bayleton™) in triadimefon technical and formulated products has been developed and subjected to a collaborative study with 7 participating collaborators. Formulations were extracted with mobile solvent and analyzed by normal phase chromatography, with 4-chlorophenyl sulfoxide as an internal standard. Collaborators were furnished with standards and samples of technical products, 50% wettable powders, and 25% wettable powders for analysis. Coefficients of variation of the values obtained on these samples were 1.42, 0.82, and 1.05%, respectively. The method has been adopted official first action.

Gas-Liquid Chromatographic Method for Analysis of Pentachloronitrobenzene Formulations: Collaborative Study

1982 ◽  
Vol 65 (1) ◽  
pp. 110-114
Author(s):  
Alan R Hanks
Keyword(s):  
Chromatographic Method ◽  
Collaborative Study ◽  
Internal Standard ◽  
Peak Height ◽  
Matched Pairs ◽  
Commercial Products ◽  
Coefficients Of Variation ◽  
Liquid Chromatographic Method ◽  
Wettable Powder ◽  
Liquid Chromatographic

Abstract A collaborative study has been conducted on a gasliquid chromatographic (GLC) method for determining pentachloronitrobenzene (PCNB) in formulations. Wettable powder, liquid, and granular matched pairs of commercial products were analyzed by 17 laboratories using peak height measurements and by 12 laboratories using integrator area measurements. Samples were dissolved in chloroform and aliquots were mixed with internal standard before GLC analysis on a 5% SE-30 column. Mean coefficients of variation for the completed study were 1.54% for integrator area measurements and 1.35% for peak height measurements. The method has been adopted official first action.

Gas-chromatographic determination of mephenytoin and desmethylmephenytoin, after off-column alkylation.

1979 ◽  
Vol 25 (1) ◽  
pp. 172-175
Author(s):  
V A Raisys ◽  
A M Zebelman ◽  
S F MacMillan
Keyword(s):  
Active Metabolite ◽  
Chromatographic Method ◽  
Seizure Control ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Peak Height ◽  
Therapeutic Concentration ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic

Abstract We describe a gas-liquid chromatographic method for determining mephenytoin and its active metabolite, desmethylmephenytoin, in human serum. 5-Methyl-5-phenylhydantoin is used as the internal standard. The method involves extraction of the drugs by adsorption onto charcoal and off-column derivatization to their pentyl derivatives. Peak height and concentration are linearly related and the day-to-day CV for therapeutic concentration is about 2 to 6%. No interferences by endogenous compounds or drugs commonly used for seizure control have been encountered.

Simultaneous determination of haloperidol and its reduced metabolite in serum and plasma by isocratic liquid chromatography with electrochemical detection.

1983 ◽  
Vol 29 (4) ◽  
pp. 624-628 ◽  
Author(s):  
E R Korpi ◽  
B H Phelps ◽  
H Granger ◽  
W H Chang ◽  
M Linnoila ◽  
...  
Keyword(s):  
Psychiatric Patients ◽  
Internal Standard ◽  
Isoamyl Alcohol ◽  
Reversed Phase ◽  
Reduced Haloperidol ◽  
Liquid Liquid Extraction ◽  
Liquid Chromatographic Method ◽  
The Central Nervous System ◽  
Liquid Chromatographic

Abstract We describe a liquid-chromatographic method for simultaneous quantification of haloperidol and its reduced metabolite in plasma and serum. Haloperidol and reduced haloperidol are concentrated from blood samples by liquid/liquid extraction into a hexane/isoamyl alcohol mixture, with chlorohaloperidol as the internal standard. For chromatographic separation we used a reversed-phase cyano-bonded column and a mobile phase of pH 6.8 phosphate buffer/acetonitrile (55/45 by vol). Haloperidol and its reduced metabolite are detected electrochemically at +0.90 V potential between the working and reference electrodes. As little as 0.5 ng per injection is detectable. Within- and between-day CVs for determinations of haloperidol and reduced haloperidol ranged from 4 to 7% each at a concentration of 10 micrograms/L. Haloperidol concentrations measured by this method correlated well with those by gas-chromatography with nitrogen-sensitive detector and by radioimmunoassay. The present method can be used to study the effects of haloperidol on the central nervous system. It is simple enough for use in clinical laboratories that are monitoring haloperidol concentrations in the blood of psychiatric patients.

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