Liquid chromatographic determination of domoic acid in shellfish products using the paralytic shellfish poison extraction procedure of the association of official analytical chemists

1989 ◽  
Vol 462 ◽  
pp. 349-356 ◽  
Author(s):  
James F. Lawrence ◽  
Claudette F. Charbonneau ◽  
Cathie Ménard ◽  
Michael A. Quilliam ◽  
P.Greig Sim
Keyword(s):  
Domoic Acid ◽  
Extraction Procedure ◽  
Chromatographic Determination ◽  
Paralytic Shellfish Poison ◽  
Paralytic Shellfish ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Liquid Chromatographic Determination of Domoic Acid in Mussels, Using AOAC Paralytic Shellfish Poison Extraction Procedure: Collaborative Study

1991 ◽  
Vol 74 (1) ◽  
pp. 68-72 ◽  
Author(s):  
James F Lawrence ◽  
Claudette F Charbonneau ◽  
Cathie Ménard
Keyword(s):  
Domoic Acid ◽  
Collaborative Study ◽  
Extraction Procedure ◽  
Chromatographic Determination ◽  
Mussel Tissue ◽  
Individual Values ◽  
Paralytic Shellfish Poison ◽  
Paralytic Shellfish ◽  
Relative Standard ◽  
Liquid Chromatographic

Abstract A liquid chromatographic method using the AOAC paralytic shellfish poison (PSP) extraction procedure for domoic acid, a marine toxin, in mussel tissue was collaboratively studied in 10 laboratories. Domoic acid is extracted by boiling the homogenized tissue for 5 min with 0.1N HCI. The mixture is cooled, diluted to a known volume, and then centrifuged. An aliquot of the supernate Is diluted, filtered, and analyzed by reverse-phase liquid chromatography with a mobile phase containing acetonitrile and water adjusted to about pH 2.5. Each collaborator received a prepared standard solution, a practice sample, and 7 randomly numbered unknown samples (1 blank mussel tissue, 1 spiked at 14.1 µg domoic acid/ g, 1 spiked at 18.9 µg/g, and duplicate samples with naturally Incurred domoic acid at 75 µ/g and at 186 µ/g). Five of the laboratories had little or no experience In domoic acid analysis. Ten of 11 laboratories completed the study and submitted results. Two Individual values out of a total of 70 were found to be outliers. Mean recovery of domoic acid from the spiked extracts was 75%. Relative standard deviations between laboratories (RSDR) ranged from 7.5 to 19.4%; wlthln-laboratory RSDs (RSDr) for the 2 blind duplicate pairs were 1.9 and 4.8%. The detection limit was about 1 fig domoic acld/g. The method has been adopted official first action by AOAC.

Gas-Liquid Chromatographic Determination of Dioxathion and Quintiofos in Organophosphorus Dip Washes

1980 ◽  
Vol 63 (1) ◽  
pp. 33-36
Author(s):  
Molly I Keating
Keyword(s):  
Solvent Extraction ◽  
Extraction Procedure ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Phosphorus Compounds ◽  
Ionization Detector ◽  
Liquid Chromatographic Determination ◽  
Gasliquid Chromatography ◽  
Liquid Chromatographic

Abstract A rapid method for the analysis of dip washes is described which eliminates the usual solvent extraction procedure. The dip wash is initially diluted with acetone and then with petroleum ether. The diluted dip wash is analyzed by gasliquid chromatography, using an alkali ionization detector sensitive to phosphorus compounds. The method was applied to the determination of dioxathion (2,3-ρ-dioxanedithiol S,S-bis(O,O-diethyl phosphorodithioate)), and quintiofos (O-ethyl O-8-quinolyl phenylphosphonothioate) dip washes. Average recoveries from fouled dip washes were 100 and 104%. GLC of these compounds with an internal standard is described, which improves the precision of the method to ±2%.

Rapid Extraction and Cleanup for Liquid Chromatographic Determination of Domoic Acid in Unsalted Seafood

1995 ◽  
Vol 78 (2) ◽  
pp. 543-554 ◽  
Author(s):  
Michael A Quilliam ◽  
Mie Xie ◽  
William R Hardstaff
Keyword(s):  
Domoic Acid ◽  
Dynamic Range ◽  
Solid Phase ◽  
Chromatographic Determination ◽  
Single Step ◽  
Shellfish Poisoning ◽  
Rapid Extraction ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract Domoic acid is the toxin responsible for incidents of amnesic shellfish poisoning. A rapid extraction and cleanup for the liquid chromatographic determination of domoic acid in unsalted seafood is reported. The method uses a single-step extraction with 50% aqueous methanol and a selective cleanup and preconcentration with strong-anion exchange, solid-phase extraction. Determination is performed by liquid chromatography with ultraviolet absorbance detection. The detection limit was 20–30 ng/g. Recoveries of 93% were achieved from 0.2 to 20 μg/g in mussel tissues. The method gave a precision of less than 3% for concentrations greater than 2 μg/g and less than 6% at 0.2 μg/g. A linear dynamic range of 104 can be achieved. The method was successfully applied to a variety of seafood products, including mussels, razor clams, crabs, and anchovies.

High-Speed Liquid Chromatographic Determination of Biphenyl Residues in Citrus Products

1975 ◽  
Vol 58 (5) ◽  
pp. 1013-1014
Author(s):  
Samuel K Reeder
Keyword(s):  
Liquid Chromatography ◽  
Rapid Method ◽  
Orange Juice ◽  
High Speed ◽  
Extraction Procedure ◽  
Chromatographic Determination ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A simple, direct, and rapid method is given for the analysis of citrus oils for the fungistat biphenyl by high-speed liquid chromatography. The method is extended to orange juice and various “dry flavors” by an extraction procedure. Analytical limits are <1 ppm without need for any cleanup or concentration steps.

Rapid Reverse Phase Liquid Chromatographic Determination of Aflatoxin M1 in Milk

1985 ◽  
Vol 68 (3) ◽  
pp. 462-465
Author(s):  
Ahmed E Yousef ◽  
Elmer H Marth
Keyword(s):  
Extraction Procedure ◽  
Chromatographic Determination ◽  
New Method ◽  
Aflatoxin M1 ◽  
Cleanup Procedure ◽  
Aoac Method ◽  
Liquid Chromatographic Determination ◽  
Phase Liquid ◽  
Liquid Chromatographic

Abstract A rapid, economical, and reliable liquid chromatographic (LC) method is described for determination of aflatoxin M, in milk. The method includes an improved AOAC extraction procedure, cleanup of the extract on a silica cartridge, and LC quantitation. Alternatively, a rapid column cleanup procedure can be used. Milk artificially spiked with aflatoxin M1 at 0.05, 0.1, and 0.5 ppb was analyzed using both new approaches as well as an AOAC method coupled with LC for quantitation of the toxin. Recovery of aflatoxin M1 by the first approach of the new method ranged between 93.4 and 99.1%, and for the alternative procedure between 92.4 and 96.8%. The AOAC method gave lower recovery (85.6-90.7%) of toxin, but the results from this method had a somewhat smaller standard deviation for replicate analyses than did results of the new method.

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