Review of Analytical Methods for the Determination of Nonylphenol and Related Compounds in Environmental Samples

1999 ◽  
Vol 34 (1) ◽  
pp. 3-36 ◽  
Author(s):  
Hing-Biu Lee
Keyword(s):  
Analytical Methods ◽  
Environmental Samples ◽  
Solid Phase ◽  
Soxhlet Extraction ◽  
Reversed Phase ◽  
Phase Liquid ◽  
Capillary Column Gas Chromatography ◽  
Preconcentration Techniques ◽  
Related Compounds

Abstract Analytical methods published in the last 20 years for the extraction, chromato-graphic separation, and quantification of alkylphenol ethoxylates (APEO) and related compounds in environmental samples are reviewed. Examples of various isolation and preconcentration techniques for water, effluent, sediment and sludge are presented. This includes procedures from the classical liquid-liquid and Soxhlet extraction to the up-to-date solid phase and supercritical fluid extraction. Chromatographic separation of APEO by normal and reversed phase liquid chromatography (LC) and capillary column gas chromatography (GC) is compared. A variety of quantification methods involving the common LC and GC detectors as well as various mass spectrometric techniques are also discussed.

Determination of Polynuclear Aromatic Hydrocarbons in Seafood by Liquid Chromatography with Fluorescence Detection

1992 ◽  
Vol 75 (5) ◽  
pp. 872-877 ◽  
Author(s):  
Gracia A Perfetti ◽  
Patricia J Nyman ◽  
Sheryl Fisher ◽  
Frank L Joe ◽  
Gregory W Diachenko
Keyword(s):  
Liquid Chromatography ◽  
Fluorescence Detection ◽  
Aromatic Hydrocarbons ◽  
Solid Phase ◽  
Reversed Phase ◽  
Polynuclear Aromatic Hydrocarbons ◽  
Matrix Interferences ◽  
Phase Liquid ◽  
Certified Values

Abstract Modification of a previously published method for determination of polynuclear aromatic hydrocarbons (PAHs) produces very clean seafood extracts in less than half the time. After alkaline digestion of the seafood, PAHs were partitioned into 1,1,2- trichlorotrifluoroethane. The resulting extract was cleaned up by solid-phase extraction on alumina, silica, and C18 adsorbents and then analyzed by gradient reversed-phase liquid chromatography with programmable fluorescence detection. Average recoveries of 12 PAHs [acenaphthene, anthracene, fluoranthene, pyrene, benz(a)anthracene, chrysene, benzo(b)fluoranthene, benzo(k)- fluoranthene, benzo(a)pyrene, dibenz(a,h)anthracene, benzo(ghi)perylene, and indeno(1,2,3-cd)pyrene] from 5 different matrixes (mussels, oysters, clams, crabmeat, and salmon) spiked at low partsper- billion levels ranged from 76 to 94%. Estimated limits of quantitation ranged from 0.01 to 0.6 ppb PAHs in extracts that were free of matrix interferences. Results of analyses of a mussels standard reference material obtained from the National Institute of Standards and Technology were in good agreement with the certified values.

scholarly journals Determination of Tylosin in Feeds by Liquid Chromatography with Solid-Phase Extraction

2004 ◽  
Vol 87 (2) ◽  
pp. 341-345 ◽  
Author(s):  
Matthew J Gramse ◽  
Paul E Jacobson ◽  
James C Selkirk
Keyword(s):  
Liquid Chromatography ◽  
Solid Phase Extraction ◽  
Solid Phase ◽  
Reversed Phase ◽  
Phase Extraction ◽  
Column Temperature ◽  
Solid Phase Extraction Cartridge ◽  
Relative Standard ◽  
Phase Liquid

Abstract A method was developed for the determination of tylosin in feeds. The method involves extraction of tylosin with methanol, concentration under a stream of nitrogen, and cleanup using Phenomenex C18 solid-phase extraction cartridge. Analyte separation and quantitation were achieved by gradient reversed-phase liquid chromatography and UV absorbance at 285 nm with a reference wavelength of 320 nm with column temperature of 45°C. Average spike recoveries for samples prepared at 4 spiking levels (22.7, 181, 907, and 1000 g/ton) were 111.0, 94.9, 96.2, and 98.6%, respectively. The overall method precision at each of the 4 spiking levels was ≤ 7.85% relative standard deviation. The limits of detection and quantitation (g/ton) were 2.16 and 7.20 g/ton, respectively.

Determination of Phenol Sulfone, Phenol Sulfoxide, and Phenol Sulfonic Acid Metabolites of Fenamiphos in Soil by Liquid Chromatography

1995 ◽  
Vol 78 (5) ◽  
pp. 1286-1293
Author(s):  
Gregory C Mattern ◽  
Gilbert D Parker ◽  
Debra L Green ◽  
Gregory L Yeutter
Keyword(s):  
Liquid Chromatography ◽  
Solid Phase Extraction ◽  
Sulfonic Acid ◽  
Solid Phase ◽  
Reversed Phase ◽  
Uv Detection ◽  
Phase Extraction ◽  
Soil Matrix ◽  
Phase Liquid

Abstract An analytical method has been developed to quantitate fenamiphos phenol sulfone, phenol sulfoxide, and phenol sulfonic acid in soil. Both control and analyte-fortified soil samples from Fresno, CA, were extracted with methanol–water (2 + 1) and partitioned with ethyl acetate. Fenamiphos phenol sulfone and phenol sulfoxide were determined by re-versed-phase liquid chromatography (LC) with UV detection at 240 nm after cleanup by silica solid-phase extraction. Fenamiphos phenol sulfonic acid was determined by reversed-phase ion-pairing LC with UV detection at 240 nm after cleanup by amino solid-phase extraction. Recoveries of fenamiphos phenol sulfoxide ranged from 88.2 to 111.0%, with an average of 97.4%. Recoveries of fenamiphos phenol sulfone ranged from 101.6 to 107.0%, with an average of 104.6%. Recoveries of fenamiphos phenol sulfonic acid ranged from 76.0 to 99.9%, with an average of 86.0%. Responses for analysis of analytes in both solvent and soil matrix were linear over the tested range of 10 to 500 ppb. Limits of determination of each analyte in soil were less than 10 ppb.

scholarly journals Chlortetracycline, Oxytetracycline, and Tetracycline in Edible Animal Tissues, Liquid Chromatographic Method: Collaborative Study

1996 ◽  
Vol 79 (2) ◽  
pp. 405-417 ◽  
Author(s):  
James D MacNeil ◽  
Valerie K Martz ◽  
Gary O Korsrud ◽  
Craig D C Salisbury ◽  
Hisao Oka ◽  
...  
Keyword(s):  
Chromatographic Method ◽  
Solid Phase ◽  
Collaborative Study ◽  
Reversed Phase ◽  
Animal Tissues ◽  
Liquid Chromatographic Method ◽  
Phase Liquid ◽  
Tetracycline Residues ◽  
Liquid Chromatographic

Abstract Thirteen laboratories analyzed samples of edible animal tissues for tetracycline residues. The method included extraction of analytes into buffer, elution from a C18 solid-phase extraction (SPE) cartridge, and reversed-phase liquid chromatographic (LC) analysis, including use of a confirmation column. An additional laboratory, using an alternative LC assay based on a different sample cleanup, also analyzed the samples. Results showed the 2 methods are comparable. The LC method for determination of cholortetracycline, oxytetracycline, and tetracycline in edible animal tissues has been adopted by AOAC INTERNATIONAL. Results from 13 laboratories indicate that the method under study provides generally better results at the higher concentrations tested than at concentrations near the detection limit and that there is less problem with interferences in muscle tissue than in kidney. The method can achieve reliable results for analytes and matrixes studied at concentrations from 0.1 to 0.6 ppm and above, depending on the analyte-matrix combination, with generally better performance to be expected with muscle than with kidney. The poorer performance for fortified samples, particularly kidney, was attributed to additional homogenization steps required to prepare these samples. Recovery of analytes from different

Analysis of 5-Vinyl-l,3-Oxazolidine-2-Thione by Liquid Chromatography

1992 ◽  
Vol 75 (3) ◽  
pp. 529-536 ◽  
Author(s):  
Alain Quinsac ◽  
Daniel Ribaillier ◽  
Patrick Rollin ◽  
Michel Dreux
Keyword(s):  
Liquid Chromatography ◽  
Solid Phase ◽  
Internal Standard ◽  
Rapeseed Meal ◽  
Reversed Phase ◽  
Mercury Acetate ◽  
Phase Liquid ◽  
Biological Environment ◽  
Liquid Chromatographic

Abstract 5-Vlnyl-1,3-oxazolldlne-2-thlone (5-VOT) Is a goltrlgenlc compound released by enzymatic degradation of progoltrln, the major glucoslnolate occurring In rapeseed meal. A liquid chromatographic (LC) method for determination of 5-VOT in a biological environment Is presented. Complete extraction of 5-VOT has been carried out by complexatlon with phenyl mercury acetate under cyclohexanlc conditions, and then by decomplexation using an aqueous sodium thlosulfate solution. These reactions displace 5-VOT from an aqueous to an organic medium, and then back again to the aqueous condition, thus assuring high selectivity of the extraction. Precise quantitation of 5-VOT Is completed in 10 mln by reversed-phase liquid chromatography using an isocratic elutlon with UV detection and a specially made synthetic Internal standard. Concentration steps by solid-phase chromatography and evaporation can be introduced In the analytic procedure to lower the detection limit of 5-VOT in the sample used from 100 to 0.5 ppb. Using sow milk samples, the method was tested by small measured additions of 5-VOT. The recovery rate of the product was very good (>97%). Different phases used to achieve a sensitive, rapid, and precise method are described.

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