Determination of Benzo(a)Pyrene and other Polynuclear Aromatic Hydrocarbons in Airborne Particulate Material by Ultrasonic Extraction and Reverse Phase High Pressure Liquid Chromatography

Abstract A simple, rapid method has been developed for the separation and determination of polynuclear aromatic hydrocarbons (PAHs) in barley malt. An ultrasonic- cyclohexane extraction method was used to separate the PAHs from ground barley malt. The cyclohexane extracts were purified by chromatography through a water-deactivated silica gel-alumina column. The eluate from the column was concentrated and purified further by partitioning between dimethyl sulfoxide (DMSO) and cyclohexane. The DMSO extract was diluted with water and the PAHs were extracted back into cyclohexane. The cyclohexane extract was washed with water, dried through sodium sulfate, and evaporated, and the resulting residue was dissolved in 80% aqueous acetonitrile-methanol (1 + 1) and subjected to reverse phase high performance liquid chromatography. Thirty barley malt samples were analyzed using this procedure. Peaks having the same retention time as the carcinogen benzo(a)pyrene were isolated from 18 of the samples, and were equivalent to trace levels ranging from <0.1 to 0.2 ppb. Average recoveries of 11 PAHs, including benzo(a)pyrene, benzo(b)fluoranthene, indeno(l,2,3-cd)pyrene, and benz(a)anthracene, added to 25 g samples at 2.5 and 5 ppb, ranged from 78 to 97%, with a mean relative standard deviation of 6.6%.

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Determination of Zearalenone in Corn by High Pressure Liquid Chromatography and Fluorescence Detection

Journal of AOAC INTERNATIONAL ◽

10.1093/jaoac/61.5.1058 ◽

1978 ◽

Vol 61 (5) ◽

pp. 1058-1062

Author(s):

George M Ware ◽

Charles W Thorpe

Keyword(s):

High Pressure ◽

Liquid Chromatography ◽

High Pressure Liquid Chromatography ◽

Fluorescence Detection ◽

Hplc Analysis ◽

Fluorescence Detector ◽

Reverse Phase

Abstract A method is reported for determining zearalenone in corn at levels as low as 10 ng/g. Samples are extracted with chloroform-water and cleaned up by liquid-liquid chromatography, and the zearalenone is detected by a fluorescence detector after separation by reverse phase high pressure liquid chromatography (HPLC). Recoveries of zearalenone added to corn at levels from 10 to 200 ng/g averaged greater than 89%. In addition, a confirmation procedure is described which involves sequential HPLC analysis of the sample and a zearalenone standard, using 4 different excitation wavelengths and comparing fluorescence responses obtained. This method was successfully applied to the analysis of 11 samples of cornmeal; zearalenone was detected in 9 of the samples at levels from 11 to 69 ng/g.

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Determination of polycyclic aromatic hydrocarbons in atmospheric particulate matter by high pressure liquid chromatography coupled with fluorescence techniques

Analytical Chemistry ◽

10.1021/ac60371a002 ◽

1976 ◽

Vol 48 (7) ◽

pp. 992-998 ◽

Cited By ~ 96

Author(s):

Marye Anne. Fox ◽

Stuart W. Staley

Keyword(s):

High Pressure ◽

Polycyclic Aromatic Hydrocarbons ◽

Liquid Chromatography ◽

Particulate Matter ◽

High Pressure Liquid Chromatography ◽

Aromatic Hydrocarbons ◽

Atmospheric Particulate Matter ◽

Fluorescence Techniques ◽

Polycyclic Aromatic

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A Simple Procedure for the Determination of Carbamazepine in Plasma by High Pressure-Liquid Chromatography

Annals of Clinical Biochemistry International Journal of Laboratory Medicine ◽

10.1177/000456327901600150 ◽

1979 ◽

Vol 16 (1-6) ◽

pp. 213-216 ◽

Cited By ~ 1

Author(s):

C. K. Johnston ◽

G. H. Lester

Keyword(s):

High Pressure ◽

Liquid Chromatography ◽

High Pressure Liquid Chromatography ◽

Mobile Phase ◽

Simple Procedure ◽

Internal Standard ◽

Reverse Phase ◽

Coefficients Of Variation ◽

Initial Results

We describe a simple, rapid procedure for the estimation of carbamazepine in plasma. Protein is precipitated, and extraction is achieved by the addition of acetonitrile containing the internal standard N-acetyltryptophan ethyl ester. Separation is by reverse-phase high-pressure liquid chromatography with an acetonitrile: water mobile phase, and detection is by UV absorption at 280 nm. Total retention time is less than 7 minutes. Initial results gave within-batch and between-batch coefficients of variation of less than 2 %, and mean recovery of 97 %. The method is free from interference by other common anticonvulsant drugs.

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