Gas Chromatographic Determination of p-Chloroaniline in a Chlorhexidine Digluconate-Containing Alcohol Foam Surgical Scrub Product

1994 ◽  
Vol 77 (3) ◽  
pp. 583-586 ◽  
Author(s):  
Walter K Gavlick ◽  
Paula K Davis
Keyword(s):  
Dynamic Range ◽  
Preparation Method ◽  
Limit Of Detection ◽  
Chromatographic Determination ◽  
Chlorhexidine Digluconate ◽  
Linear Dynamic Range ◽  
Sample Preparation Method ◽  
Flame Ionization ◽  
Limit Of Quantitation

Abstract A gas chromatographic (GC) method with flame ionization detection was developed to separate and quantitate p-chloroaniline (PCA) from other components in a chlorhexidine digluconate (CHG)-containing alcohol foam surgical scrub product. A simple sample preparation method was developed in which 1-butanol was used to dissolve the foam and precipitate the CHG, which otherwise would interfere with the GC analysis. The method was validated with respect to linear dynamic range, precision, accuracy, selectivity, limit of detection, and limit of quantitation.

Gas-chromatographic determination of ethylene glycol in serum.

1982 ◽  
Vol 28 (1) ◽  
pp. 75-78 ◽  
Author(s):  
W H Porter ◽  
A Auansakul
Keyword(s):  
Ethylene Glycol ◽  
Dynamic Range ◽  
Limit Of Detection ◽  
Chromatographic Determination ◽  
Good Precision ◽  
Linear Dynamic Range ◽  
Linear Dynamic ◽  
Analytical Recovery ◽  
Chromatographic Procedure

Abstract We describe a new gas-chromatographic procedure for ethylene glycol in serum, determined as the cyclic phenylboronate ester. The method is rapid, requires only 100 microL of serum, and either an OV-1 or an OV-17 column is used. The linear dynamic range extends to at least 5000 mg/L, with a lower limit of detection of 10 mg/L. Analytical recovery of ethylene glycol from serum averaged 97% (95-101%) over the concentration range of 250-5000 mg/L. The method demonstrates good precision, with CVs less than 2.5%, over the concentration range 500-2000 mg/L.

scholarly journals Liquid Chromatographic Determination of α-Solasonine in Frozen Green Peas as an Indicator of the Presence of Nightshade Berries

2003 ◽  
Vol 86 (4) ◽  
pp. 759-763 ◽  
Author(s):  
Peter Cavlovic ◽  
Mohan Mankotia ◽  
Peter Pantazopoulos ◽  
Peter M Scott
Keyword(s):  
Limit Of Detection ◽  
Chromatographic Determination ◽  
Solanum Nigrum ◽  
Expanded Uncertainty ◽  
Method Performance ◽  
Limit Of Quantitation ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
Green Peas

Abstract Nightshade berries containing glycoalkaloids can be a contaminant in green peas. Methodology was developed to detect this contamination. The glycoalkaloid α-solasonine was extracted from frozen green peas with 1% (v/v) acetic acid, cleaned up on a C18 cartridge, and determined by liquid chromatography with UV detection at 200 nm. Method performance characteristics for the determination of α-solasonine include linearity from 140 to 1500 ng injected (r = 0.9996–0.9999); recovery ranging from 68 to 79%; limit of quantitation (LOQ) = 4.5 ppm (280 ng standard), and limit of detection = 0.64 ppm (40 ng standard). At the LOQ, the expanded uncertainty at 95% confidence was 0.38 × the reported value. The method was applied to the detection of α-solasonine in frozen green peas in a 2-year study of 60 samples of frozen green peas from Ontario, Canada. None of the samples contained α-solasonine. No unripe berries of Solanum nigrum were detected visually in the samples.

Gas Chromatographic Determination of Pentachlorophenol in Gelatin

1984 ◽  
Vol 67 (2) ◽  
pp. 275-277
Author(s):  
Arnold P Borsetti ◽  
Lee S Thurston
Keyword(s):  
Gas Chromatography ◽  
Liquid Phase ◽  
Electron Capture ◽  
Limit Of Detection ◽  
Direct Determination ◽  
Chromatographic Determination ◽  
Gelatin Matrix ◽  
Limit Of Quantitation ◽  
Acetate Derivative

Abstract A method is described for the determination of pentachlorophenol (PCP) in gelatin. The method employs acid and heat to hydrolyze the gelatin matrix, a base partition and wash for separation and cleanup, and a reacidification and extraction with hexane for direct determination of PCP, without preparation of a derivative, using gas chromatography (GC) with a 1% SP-1240DA liquid phase and a 63Ni electron capture detector. Recoveries averaged 106% for fortifications between 0.02 and 1.0 ppm. The limit of quantitation is 20 ppb. The limit of detection is 4-6 ppb. The method, which has undergone a successful intralaboratory trial, is simple and rapid, and requires only general laboratory reagents and equipment. GC of the acetate derivative of PCP is used for confirmation of identity.

Liquid Chromatographic Determination of 5-(Methylamino)-2-Phenyl-4-[3-(Trifluoromethyl)phenyl]-3-(2H)-Furanone in Soil

1990 ◽  
Vol 73 (2) ◽  
pp. 298-299
Author(s):  
Thomas C Mueller ◽  
Philip A Banks ◽  
Parshall B Bush ◽  
William C Steen
Keyword(s):  
Limit Of Detection ◽  
Chromatographic Determination ◽  
Soil Samples ◽  
Soil Types ◽  
Liquid Chromatographic Separation ◽  
Relative Standard ◽  
Limit Of Quantitation ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A rapid, sensitive method is described for the determination of5-(methylamlno)-2-phenyl-4-[3-(trlfluoromethyl)phenyl]-3- (2M)-furanone (RE-40885) concentrations in 3 soil types. The method consists of extraction of soil samples with methanol, filtration, liquid chromatographic separation of methanolsoluble components using a C18 column, and UV detection at 275 nm. Recoveries were 94, 96, and 94% from the Greenville, Cecil, and Dothan soils, respectively. Average relative standard deviation was 8.0% in the Greenville soil. The qualitative limit of detection was 20 ppb and the limit of quantitation was 40 ppb in 25 g soil samples.

Capillary Gas Chromatographic Determination with Electron Capture Detector of β-Propiolactone in Biological Materials

1991 ◽  
Vol 74 (4) ◽  
pp. 595-599
Author(s):  
Aziz Geahchan ◽  
Bruno Fouillet ◽  
Paul Chambon ◽  
Renee Chambon ◽  
Bahia Nouri
Keyword(s):  
Electron Capture ◽  
Limit Of Detection ◽  
Chromatographic Determination ◽  
Biological Materials ◽  
Electron Capture Detector ◽  
Detector Response ◽  
Limit Of Quantitation ◽  
Low Levels ◽  
Ppm Level

Abstract A method has been developed for the determination of β- propiolactone by derivatizing it to the volatile N-hexyl-3- heptafluorobutanoyloxypropanamide, which can be separated and Identified by a capillary CP-Sil 8 column, and detected by an electron capture detector (ECD). First, β- propiolactone is reacted with N-hexylamine to yield N-hexyl- 3-hydroxypropanamide. The fluorobutanoyl ester derivative is next prepared by using heptafluorobutyrlc acid anhydride in the presence of trimethylamine. The method Is very sensitive, simple, and specific, and can be used to detect and quantitate residual β-propiolactone In Iyophilized biological materials. The limit of detection is 0.2 ppm β-proplolactone in a 50 mg sample; however, because of variability at low levels, the limit of quantitation is 1 ppm. Detector response was linear for 2-500 ng β-propiolactone. Recoveries were 98% or greater from Iyophilized vaccines spiked at the 2-20 ppm level. No side products or interference peaks were observed in the derivatization reaction.

scholarly journals Application of a Reliable LC-MS/MS Method for Determination of Rizatriptan in Healthy Subject Samples: Demonstration of Assay Reproducibility by Incurred Sample Reanalysis

2012 ◽  
Vol 2012 ◽  
pp. 1-10 ◽  
Author(s):  
Dinesh S. Patel ◽  
Naveen Sharma ◽  
Mukesh C. Patel ◽  
Bhavin N. Patel ◽  
Pranav S. Shrivastav ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Quality Control ◽  
Tandem Mass Spectrometry ◽  
Human Plasma ◽  
Dynamic Range ◽  
Limit Of Detection ◽  
Multiple Reaction Monitoring ◽  
Tandem Mass ◽  
Limit Of Quantitation

A reliable, rapid, and selective liquid chromatography-tandem mass spectrometry (LC-MS/MS) assay has been proposed for the determination of rizatriptan in human plasma using sumatriptan as internal standard (IS). The analyte and IS were extracted from 300 μL human plasma via liquid-liquid extraction and the chromatography was achieved on Hypurity C18 (50 mm × 4.6 mm, 5 μm) column under isocratic conditions. Detection of rizatriptan and IS was done by tandem mass spectrometry, operating in positive ionization and multiple-reaction monitoring mode. The limit of detection and lower limit of quantitation of the method were 0.04 and 0.20 ng/mL, respectively, with a linear dynamic range of 0.20–60.0 ng/mL. The intrabatch and interbatch precision (% CV) was ≤8.4% while the mean extraction recovery was >78% across quality control levels. Bench top stability, freeze and thaw stability, processed sample stability, and long-term stability in plasma were evaluated at two quality control levels. It was successfully applied to a bioequivalence study of 10 mg rizatriptan orally disintegrating tablet formulation in 40 and 32 healthy Indian male subjects under fasting and fed conditions, respectively. The reproducibility in the measurement of study data was demonstrated by reanalysis of 254 incurred samples.

scholarly journals Liquid Chromatographic Determination of Nicarbazin in Feeds

2000 ◽  
Vol 83 (5) ◽  
pp. 1027-1038 ◽  
Author(s):  
Beverly J Krabel ◽  
David A Dickson ◽  
Alan G Zimmermann ◽  
Mark R Coleman
Keyword(s):  
Limit Of Detection ◽  
Chromatographic Determination ◽  
Reversed Phase ◽  
Linear Range ◽  
Limit Of Quantitation ◽  
Standard Linear ◽  
Sample Recovery ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A new liquid chromatographic method has been developed for determination of nicarbazin in feeds. Approximately 40 g feed is extracted with 200 mL acetonitrile–water (80 + 20, v/v). An aliquot of the extract is filtered and assayed using a reversed-phase isocratic method that measures the 4,4′–dinitrocarbanilide moiety of nicarbazin at a wavelength of 340 nm. For medicated feeds, the method uses a standard linear range of 5 to 100 μg/mL. For lower levels, a linear range of 50 to 150 ng/mL can be used. The method has a limit of detection of 250 ng/g and a limit of quantitation of 500 ng/g in a 40 g feed sample. Recovery was 99.1%, with a range of 95.2 to 101.8%. In the typical U.S. dosing range of 27 to 113.5 g/ton, the precision of the method based on one analyst, one day, and 2 weighings ranged from 2.8% (113.5 g/ton) to 4.7% (27 g/ton).

scholarly journals Spectrophotometric Determination of Phenylephrine Hydrochloride in Pharmaceuticals by Flow Injection Analysis Exploiting the Reaction with Potassium Ferricyanide and 4-Aminoantipyrine

2002 ◽  
Vol 85 (4) ◽  
pp. 875-878 ◽  
Author(s):  
José R C Rocha ◽  
Cristiane X Galhardo ◽  
Maria Auxiliadora E Natividade ◽  
Jorge C Masini
Keyword(s):  
Flow Injection ◽  
Flow Injection Analysis ◽  
Dynamic Range ◽  
Limit Of Detection ◽  
Condensation Product ◽  
Potassium Ferricyanide ◽  
Linear Dynamic Range ◽  
Phenylephrine Hydrochloride ◽  
Nasal Decongestant

Abstract This paper presents a method for the determination of phenylephrine hydrochloride in pharmaceuticals by spectrophotometric flow injection analysis exploiting the reaction with potassium ferricyanide and 4-aminoantipyrine, which leads to the formation of a condensation product with strong absorptivity at 500 nm. The linear dynamic range was between 0.95 and 9 mg/L, with a limit of detection of 0.2 mg/L and a sampling throughput of 120 samples per hour. The method was applied to eyewashes and nasal decongestant liquid medicines.

scholarly journals Determination of Glycerin from a Marketed Personal Care Product Using Gas Chromatography

2015 ◽  
Vol 2015 ◽  
pp. 1-5
Author(s):  
Amit Kumar De ◽  
Partha Pratim Chowdhury ◽  
Shyama Prasad Chattopadhyay
Keyword(s):  
Limit Of Detection ◽  
Packed Column ◽  
Chromatographic Technique ◽  
Undecylenic Acid ◽  
Personal Care Product ◽  
Flame Ionization ◽  
Limit Of Quantitation ◽  
Complex Sample ◽  
Sample Preparation Procedure

The current study presents a packed column gas chromatographic technique for the estimation of glycerin using a flame ionization detector from a marketed hair tonic in presence of resorcinol, ethanol, biotin, keratin hydrolysate, undecylenic acid alkylolamide (hyalkyl HBU), D-biotin, nicotinic acid, and polyvinylpyrrolidone. The validation studies show the proposed method to be specific, sensitive, precise, and accurate. The method is found to be linear in the concentration range 1.25 mg/mL to 10.02 mg/mL with r2 value 0.99. The limit of detection and the limit of quantitation were 0.01 mg/mL and 0.05 mg/mL, respectively. The method does not involve any complex sample preparation procedure and is therefore suitable for regular analysis of glycerin from marketed hair tonic.

Surfactant-less water emulsion based dispersive liquid–liquid microextraction for determination of organophosphorus pesticides in aqueous samples

2015 ◽  
Vol 7 (18) ◽  
pp. 7899-7906 ◽  
Author(s):  
Mir Ali Farajzadeh ◽  
Mohammad Reza Afshar Mogaddam ◽  
Leili Esrafili
Keyword(s):  
Preparation Method ◽  
Organophosphorus Pesticides ◽  
Aqueous Samples ◽  
Sample Preparation Method ◽  
Water Emulsion ◽  
Flame Ionization ◽  
Dispersive Liquid Liquid Microextraction ◽  
Extraction Preconcentration ◽  
Liquid Microextraction

A sample preparation method, surfactant-less water emulsion based dispersive liquid–liquid microextraction coupled with gas chromatography-flame ionization detection, has been developed for the extraction, preconcentration and determination of some organophosphorus pesticides.

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