Determination of propranolol in plasma by radial compression liquid chromatography with fluorometric detection.

1985 ◽  
Vol 31 (7) ◽  
pp. 1196-1197 ◽  
Author(s):  
A el-Yazigi ◽  
C R Martin
Keyword(s):  
Internal Standard ◽  
Fluorometric Detection ◽  
Radial Compression ◽  
Monobasic Sodium Phosphate ◽  
Routine Monitoring ◽  
Micron Particle ◽  
One Step ◽  
Flow Through ◽  
Liquid Chromatographic

Abstract This radial compression liquid-chromatographic assay for propranolol in plasma is rapid, reproducible, and suitable for use in routine monitoring. A 10-micron particle, 8 mm X 10 cm CN cartridge is used in conjunction with a radial compression separation system. The mobile phase is monobasic sodium phosphate (pH 3) solution/methanol/acetonitrile (760/84/156 by vol), the flow rate 6 mL/min. Propranolol was detected by use of a spectrofluorometer equipped with a 20-microL flow-through cell, at excitation and emission wavelengths of 250 and 336 nm. The retention times for propranolol and metoprolol (the internal standard) are 3.13 and 1.42 min, respectively. A one-step extraction with chloroform yields "clean" chromatograms, with greater than 90% of the drug being analytically accounted for. Under these conditions, results are precise and accurate. Currently we are using this method to monitor propranolol in hypertensive neonates. Data on changes in the concentrations of propranolol in plasma with time are presented for one such patient.

Determination of Neomycin in Animal Tissues, Using Ion-Pair Liquid Chromatography with Fluorometric Detection

1985 ◽  
Vol 68 (1) ◽  
pp. 29-36
Author(s):  
Badar Shaikh ◽  
Edward H Allen ◽  
John C Gridley
Keyword(s):  
Mobile Phase ◽  
Potassium Phosphate ◽  
Internal Standard ◽  
Ion Pair ◽  
Fluorometric Detection ◽  
Animal Tissues ◽  
Potassium Phosphate Buffer ◽  
Reverse Phase ◽  
Liquid Chromatographic

Abstract A liquid chromatographic (LC) method is described for the determination of neomycin in animal tissues. Tissues are homogenized in 0.2M potassium phosphate buffer (pH 8.0); the homogenate is centrifuged, and the supernate is heated to precipitate the protein. The heat-deproteinated extract is acidified to pH 3.5-4 and directly analyzed by LC. The LC method consists of an ion-pairing mobile phase, a reverse phase ODS column, post-column derivatization with o-phthalaldehyde reagent, and fluorometric detection. The LC method uses paromomycin as an internal standard, and separates neomycin from streptomycin or dihydrostreptomycin because they have different retention times. The LC column separates neomycin in 25 min; the detection limit is about 3.5 ng neomycin. The overall recovery of neomycin from kidney tissues spiked at 1-30 ppm was 96% with a 9.0% coefficient of variation. The method was also applied to muscle tissue.

Liquid Chromatographic Determination of Fluorescent Derivatives of Six Sulfonamides in Bovine Serum and Milk

1995 ◽  
Vol 78 (3) ◽  
pp. 674-678 ◽  
Author(s):  
Chin-En Tsai ◽  
Fusao Kondo
Keyword(s):  
Bovine Serum ◽  
Potassium Phosphate ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Fluorometric Detection ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
Derivatives Of ◽  
Fluorescent Derivatives

Abstract A rapid and sensitive liquid chromatographic (LC) method with fluorometric detection was developed to detect sulfadiazine, sulfathiazole, sulfamethazine, sulfamonomethoxine, sulfamethoxazole, and sulfadimethoxine residues in bovine serum and milk. p-Aminobenzoic acid (PABA) was added as an internal standard. The sulfonamides were extracted from samples and derivatized with fluorescamine, and 50 μL was injected into a NovaPak C18 LC column and eluted with acetonitrile– 10 mM potassium phosphate (30 + 70, v/v). The sulfonamides were detected fluorometrically (excitation, 390 nm; emission, 475 nm), and their retention times ranged from 6.2 to 16.5 min without interference from coextractives. The detection limit for standard sulfonamide solution was 0.1 ng/mL; the calibration curves were linear between 1 and 100 ng/mL in the presence of PABA as internal standard. Recovery rates of sulfonamides from spiked samples (1 and 10 ppb) were 95.4–107.2 and 81.4–89.6% for serum and 80.7–91.1 and 62.6–84.1% for milk, respectively.

Improved assay for etoposide in plasma by radial-compression liquid chromatography with electrochemical detection.

1987 ◽  
Vol 33 (6) ◽  
pp. 803-805 ◽  
Author(s):  
A el-Yazigi ◽  
C R Martin
Keyword(s):  
Cancer Patients ◽  
Mobile Phase ◽  
Internal Standard ◽  
Phosphate Solution ◽  
Radial Compression ◽  
Separation System ◽  
Electrochemical Detector ◽  
Liquid Chromatographic Method ◽  
Micron Particle ◽  
Liquid Chromatographic

Abstract We describe a rapid, sensitive, and expedient radial-compression liquid-chromatographic method for routine quantification of etoposide (VP-16-213) in plasma of cancer patients undergoing chemotherapy with this agent. Teniposide was used as the internal standard. The mobile phase was a mixture of 10 mmol/L phosphate solution and methanol (50.7/49.3, by vol), adjusted to pH 3 with phosphoric acid. The flow rate was 2 mL/min. We used a 5-micron particle size C18 cartridge with a radial-compression separation system. The effluent was monitored with an electrochemical detector. Plasma samples are extracted with chloroform and the chloroform is evaporated. The residue, reconstituted in mobile phase, is injected onto the cartridge. Assay results were linearly related to concentration (r greater than 0.9944) over the range examined, 0.010-28.0 mg/L. The intra-run CV was less than 4.4%, and we encountered no interference from anticancer drugs or other compounds. We present data for plasma sampled at different intervals from two cancer patients being infused with etoposide.

Development and Validation of an LC-MS/MS Method for Simultaneous Determination of Canagliflozin and Metformin HCl in Rat Plasma and its Application

2020 ◽  
Vol 16 (6) ◽  
pp. 752-762
Author(s):  
Vivek Nalawade ◽  
Vaibhav A. Dixit ◽  
Amisha Vora ◽  
Himashu Zade
Keyword(s):  
Internal Standard ◽  
Rat Plasma ◽  
Precipitation Method ◽  
Herbal Extracts ◽  
One Step ◽  
Precision And Accuracy ◽  
Development And Validation ◽  
The Impact ◽  
Metformin Hcl

Background: Food and herbal extracts rich in Quercetin (QRT) are often self-medicated by diabetics and can potentially alter the pharmacokinetics (PK) of Metformin HCl (MET) and Canagliflozin (CNG) leading to food or herb-drug interactions and reduced therapeutic efficacy. However, the impact of these flavonoids on the pharmacokinetic behaviour of MET and CNG is mostly unknown. Methods: A simple one-step protein precipitation method was developed for the determination of MET and CNG from rat plasma. The mobile phase chosen was MeOH 65% and 35% water containing 0.1% formic acid at a flow rate of 1mL/min. Results: The retention time of MET, internal standard (Valsartan) and CNG was 1.83, 6.2 and 8.2 min, respectively. The method was found to be linear in the range of 200 - 8000 ng/mL for CNG and 100 = 4000 ng/ml for MET. Precision and accuracy of the method were below 20% at LLOQ and below 15% for LQC, MQC, and HQC. Conclusion: The method was successfully applied for the determination of PK of MET and CNG by using 100 μL of rat plasma. QRT co-administration affects the PK parameters of MET and CNG. This alteration in PK parameters might be of significant use for clinicians and patients.

scholarly journals Determination of Finasteride in Tablets by High Performance Liquid Chromatography

2007 ◽  
Vol 4 (1) ◽  
pp. 109-116 ◽  
Author(s):  
K. Basavaiah ◽  
B. C. Somashekar
Keyword(s):  
High Performance ◽  
Internal Standard ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Calibration Graph ◽  
Official Method ◽  
Pharmaceutical Dosage Forms ◽  
Bulk Drug ◽  
Liquid Chromatographic

A rapid, highly sensitive high performance liquid chromatographic method has been developed for the determination of finasteride(FNS) in bulk drug and in tablets. FNS was eluted from a ODS C18reversed phase column at laboratory temperature (30 ± 2°C) with a mobile phase consisting of methanol and water (80+20) at a flow rate of 1 mL min-1with UV detection at 225 nm. The retention time was ∼ 6.1 min and each analysis took not more than 10 min. Quantitation was achieved by measurement of peak area without using any internal standard. Calibration graph was linear from 2.0 to 30 μg mL-1with limits of detection (LOD) and quantification (LOQ) being 0.2 and 0.6 μg mL-1, respectively. The method was validated according to the current ICH guidelines. Within-day co efficients of variation (CV) ranged from 0.31 to 0.69% and between-day CV were in the range 1.2-3.2%. Recovery of FNS from the pharmaceutical dosage forms ranged from 97.89 – 102.9 with CV of 1.41-4.13%. The developed method was compared with the official method for FNS determination in its tablet forms.

scholarly journals Isocratic High-Performance Liquid Chromatographic Method with Ultraviolet Detection for Simultaneous Determination of Levels of Voriconazole and Itraconazole and Its Hydroxy Metabolite in Human Serum

2005 ◽  
Vol 49 (8) ◽  
pp. 3569-3571 ◽  
Author(s):  
GholamAli Khoschsorur ◽  
Franz Fruehwirth ◽  
Sieglinde Zelzer
Keyword(s):  
Human Serum ◽  
Simultaneous Determination ◽  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Specific Method ◽  
Minimum Detectable Concentration ◽  
Detectable Concentration ◽  
One Step ◽  
Liquid Chromatographic

ABSTRACT A simple, specific method is presented for simultaneous determination of voriconazole and itraconazole and its metabolite, hydroxyitraconazole, in human serum using one-step liquid-liquid extraction and high-performance liquid chromatography. Linearity tests ranged from 0.1 to 8.0 μg/ml; the minimum detectable concentration was 0.03 μg/ml.

scholarly journals High-performance liquid chromatographic determination of famotidine in human plasma using solid-phase column extraction

2003 ◽  
Vol 68 (11) ◽  
pp. 883-892 ◽  
Author(s):  
Dragica Zendelovska ◽  
Trajce Stafilov
Keyword(s):  
Human Plasma ◽  
High Performance ◽  
Solid Phase ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
High Performance Liquid Chromatographic ◽  
Water Ph ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

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.

Improved liquid-chromatographic determination of haloperidol in plasma.

1984 ◽  
Vol 30 (7) ◽  
pp. 1228-1230 ◽  
Author(s):  
A K Dhar ◽  
H Kutt
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Room Temperature ◽  
Internal Standard ◽  
Isoamyl Alcohol ◽  
Chromatographic Determination ◽  
Reversed Phase ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

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).

Liquid Chromatographic Determination of Diazepam in Tablets: Collaborative Study

1985 ◽  
Vol 68 (3) ◽  
pp. 545-546
Author(s):  
Michael Tsougros
Keyword(s):  
Collaborative Study ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Reverse Phase ◽  
Photometric Detection ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic Determination ◽  
The Mean ◽  
Liquid Chromatographic

Abstract A stability indicating liquid chromatographic method for the determination of diazepam in tablets was collaboratively studied by 6 laboratories. The method uses a Cig reverse phase column, a methanolwater mobile phase, p-tolualdehyde as the internal standard, and photometric detection at 254 nm. The collaborators were supplied with a synthetic tablet powder and 3 commercial tablet samples. The mean recovery of diazepam from the synthetic tablet powder was 100.2%. For all samples analyzed, the coefficient of variation was < 1.5%. The method has been adopted official first action.

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