Drug Quality Assessment Methods. I. Gas-Liquid Chromatographic Assay and Identification of Seven Barbiturates

1982 ◽  
Vol 65 (5) ◽  
pp. 1054-1058
Author(s):  
Donald B Black ◽  
Halina Kolasinski ◽  
Edward G Lovering ◽  
James R Watson
Keyword(s):  
Quality Assessment ◽  
Rapid Assessment ◽  
Internal Standard ◽  
Assessment Methods ◽  
Drug Quality ◽  
Aqueous Mixture ◽  
Assay Methods ◽  
Tablet Formulations ◽  
Liquid Chromatographic ◽  
Good Agreement

Abstract A gas-liquid chromatographic (GLC) procedure has been developed for the assay and identification of amobarbital, butabarbital, heptabarbital, mephobarbital, pentobarbital, phenobarbital, and secobarbital in single component capsule, elixir, injectable, suppository, and tablet formulations. After extraction into chloroform from an acidified aqueous mixture of the product, the drug is eluted isothermally from a methylphenylsilicone GLC column at 210 or 240°C and quantitated relative to thiamylal internal standard. Results were in good agreement with those obtained using pharmacopeial assay methods. The method is suitable for the rapid assessment of commercial formulations.

Gas-Liquid Chromatographic-Thermal Energy Analyzer Method for N-Nitrosodiethanolamine in Cosmetics

1981 ◽  
Vol 64 (6) ◽  
pp. 1474-1478
Author(s):  
Donald B Black ◽  
Robert C Lawrence ◽  
Edward G Lovering ◽  
James R Watson
Keyword(s):  
Thermal Energy ◽  
Room Temperature ◽  
Internal Standard ◽  
Ethylene Dichloride ◽  
Gas Liquid Chromatography ◽  
Energy Analyzer ◽  
Cosmetic Products ◽  
Aqueous Mixture ◽  
Aqueous Layer ◽  
Liquid Chromatographic

Abstract A gas-liquid chromatography-thermal energy analyzer (GLC-TEA) method has been developed for the quantitation of N-nitrosodiethanolamine (NDELA) in a variety of cosmetic products. Samples are cleaned up by a preliminary shakeout of an aqueous mixture of the cosmetic with ethylene dichloride, followed by removal of other polar and nonpolar constituents from the aqueous layer with commercial extraction columns, separation cartridges, and selected solvents. Common transnitrosating 1,3-diol preservatives sometimes found in cosmetics were eliminated after conversion to less polar cyclic boronates. The isolated NDELA fraction was trimethylsilylated at room temperature and the product was subjected to GLC-TEA, with N, N’-dinitrosopiperazine (DNPiz) used as the internal standard. Recoveries of NDELA from spiked samples usually ranged from 60 to 90%. The limit of detectability was about 5-10 ppb. The identity of NDELA was confirmed by GLC-mass spectrometry.

Liquid Chromatographic Determination of Acids and Sugars in Homolactic Cucumber Fermentations

1989 ◽  
Vol 72 (1) ◽  
pp. 52-55
Author(s):  
Maria Jesus Lázaro ◽  
Elvira Carbonell ◽  
Maria Concepcion Aristoy ◽  
Jose SafÓn ◽  
Miguel Rodrigo
Keyword(s):  
Internal Standard ◽  
Chromatographic Determination ◽  
High Yield ◽  
Column Temperature ◽  
In Series ◽  
Liquid Chromatographic Determination ◽  
Standard Values ◽  
Liquid Chromatographic ◽  
Good Agreement

Abstract A rapid, high yield, and quantitative method for determination of sugars (glucose and fructose) and acids (malic, lactic, acetic, and citric) in fresh and fermented cucumber juices is described; the procedure solves the fructose and malic acid coelution problem. Samples are prepared by passing the juice directly through a disposable C18 cartridge. Compounds are separated by liquid chromatography on an Aminex HPX-87H chromatographic column, with 0.013N H2S04 as mobile phase in the isocratic mode at 0.6 mL/min flow rate and 60°C column temperature. Compounds are then detected and quantitated by using ultraviolet and refractive index detectors connected in series, and comparing with succinic acid as internal standard. Values for both fresh and fermented cucumber juices were in good agreement with literature data.

High Pressure Liquid Chromatographic Determination of Sulfisoxazole in Pharmaceuticals and Separation Patterns of Other Sulfonamides

1981 ◽  
Vol 64 (4) ◽  
pp. 851-854
Author(s):  
Robert W Roos
Keyword(s):  
High Pressure ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
High Pressure Liquid Chromatographic ◽  
Liquid Chromatographic Method ◽  
Acetic Acid Water ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
Good Agreement

Abstract A high pressure liquid chromatographic method has been developed for the identification and determination of sulf isoxazole in tablet, liquid, and ointment dosage forms. The method specifies a µBondapak C18 column, an acetonitrile-acetic acid-water (22.5 + 1 + 76.5) mobile phase, and ultraviolet detection at 254 nm. For quantitative purposes, sulfabenzamide is used as an internal standard. Commercial preparations were analyzed by the proposed method and results were compared with those obtained by the U.S. Pharmacopeia XIX and National Formulary XIV methods; good agreement was obtained. The elution behaviors of 19 additional sulfonamides were also established to verify the specificity of the proposed method for sulfisoxazole. These elutions patterns show potential for separation and identification of all 20 sulfonamides

Overview on Image Quality Assessment Methods

2010 ◽  
Vol 2010 (1) ◽  
pp. 219-226 ◽  
Author(s):  
Gang-yi Jiang ◽  
Da-jiang Huang ◽  
Xu Wang ◽  
Mei Yu
Keyword(s):  
Image Quality ◽  
Quality Assessment ◽  
Image Quality Assessment ◽  
Assessment Methods

scholarly journals A Simple and Sensitive HPLC Method for Simultaneous Analysis of Nabumetone and Paracetamol in Pharmaceutical Formulations

2011 ◽  
Vol 8 (s1) ◽  
pp. S41-S46
Author(s):  
Prafulla Kumar Sahu ◽  
M. Mathrusri Annapurna ◽  
Dillipkumar Sahoo
Keyword(s):  
High Performance ◽  
Internal Standard ◽  
Pharmaceutical Formulations ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Aqueous Acetic Acid ◽  
Linear Calibration ◽  
Acceptance Range ◽  
Liquid Chromatographic

This paper describes a high-performance liquid chromatographic method for simultaneous estimation of nabumetone and paracetamol in binary mixture. The method was based on RP-HPLC separation and quantitation of the two drugs on hypersil C-18 column (250 mm × 4.6 mm) using a mobile phase consisting of acetonitrile and 0.05% aqueous acetic acid (70:30v/v) at flow rate of 1 mL min-1. Quantitation was achieved with PDA detector at 238 nm based on peak area with linear calibration curves at concentration ranges 5-25 µg mL-1for both the drugs. Naproxen sodium was used as internal standard. The method has been successively applied to pharmaceutical formulation. No chromatographic interference from the tablet excipients was found. The method was validated in terms of precision, robustness, recovery and limits of detection and quantitation. The intra and inter-day precision and accuracy values were in the acceptance range as per ICH guidelines.

Sign in / Sign up

Export Citation Format

Share Document