scholarly journals Sensitive determination of domoic acid in mussel tissue using dansyl chloride derivatization and liquid chromatography-mass spectrometry

2015 ◽  
Vol 7 (3) ◽  
pp. 1000-1007 ◽  
Author(s):  
Daniel G. Beach ◽  
Hechun Liu ◽  
Michael A. Quilliam
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Domoic Acid ◽  
New Method ◽  
Liquid Chromatography Mass Spectrometry ◽  
Shellfish Poisoning ◽  
Mussel Tissue ◽  
Amnesic Shellfish Poisoning ◽  
Sensitive Determination

This paper describes a new method for sensitive determination of domoic acid (DA), the causative toxin of amnesic shellfish poisoning (ASP), in shellfish.

scholarly journals NEW METHOD DEVELOPMENT AND VALIDATION FOR THE DETERMINATION OF FEBUXOSTAT IN HUMAN PLASMA BY LIQUID CHROMATOGRAPHY–MASS SPECTROMETRY

2016 ◽  
Vol 8 (9) ◽  
pp. 61 ◽  
Author(s):  
Narottam Pal ◽  
Avanapu Srinivasa Rao ◽  
Pigilli Ravikumar
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Human Plasma ◽  
Method Development ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
New Method ◽  
Liquid Chromatography Mass Spectrometry ◽  
Chromatography Mass Spectrometry

<p><strong>Objective</strong>:<strong> </strong>To develop a new method and validate the same for the determination of Febuxostat (FBS) in human plasma by liquid chromatography–mass spectrometry (LCMS).</p><p><strong>Methods</strong>:<strong> </strong>The present method utilized reversed-phase high-performance liquid chromatography with tandem mass spectroscopy. Febuxostat D9 (FBS D9) was used as internal standard (IS). The analyte and internal standard were separated from human plasma by using solid phase extraction method. Zorbax Eclipse XDB, C<sub>8</sub>, 100 mm x 4.6 mm, 3.5 µm column was used and HPLC grade acetonitrile, 5 millimolar (mM) ammonium format (80: 20, v/v) as mobile phase, detected by mass spectrometry operating in positive ion and multiple reaction monitoring modes.</p><p><strong>Results</strong>:<strong> </strong>The parent and production transitions for FBS and internal standard were at m/z 317.1→261.0 and 326.1→262.0 respectively. The method was validated for system suitability, specificity, carryover effect, linearity, precision, accuracy, matrix effect, sensitivity and stability. The linearity range was from 20.131 ng/ml to10015. 534 ng/ml with a correlation coefficient of 0.999. Precision results (%CV) across six quality control samples were within the limit. The percentage recovery of FBS and internal standard from matrix samples was found to be 76.57% and 75.03% respectively.</p><p><strong>Conclusion</strong>:<strong> </strong>Present study describes new LC-MS method for the quantification of FBS in a pharmaceutical formulation. According to validation results, it was found to be a simple, sensitive, accurate and precise method and also free from any kind of interference. Therefore the proposed analytical method can be used for routine analysis for the estimation of FBS in its formulation.</p>

scholarly journals Determination of Domoic Acid in Japanese Mussels by Enzyme Immunoassay

2000 ◽  
Vol 83 (6) ◽  
pp. 1384-1386 ◽  
Author(s):  
Kentaro Kawatsu ◽  
Yonekazu Hamano ◽  
Tamao Noguchi
Keyword(s):  
Monoclonal Antibody ◽  
Enzyme Immunoassay ◽  
Domoic Acid ◽  
Immunoaffinity Chromatography ◽  
Shellfish Poisoning ◽  
Mussel Tissue ◽  
Blue Mussels ◽  
Amnesic Shellfish Poisoning ◽  
Low Concentrations

Abstract Ten samples of commercial blue mussels (Mytilus edulis) from Japan were analyzed for domoic acid by an indirect competitive enzyme immunoassay (idc–EIA) based on an anti-domoic acid monoclonal antibody. Domoic acid was found in all samples at low concentrations (0.11–1.81 ng/g mussel tissue). The presence of domoic acid was confirmed by liquid chromatography coupled with immunoaffinity chromatography using an anti-domoic acid monoclonal antibody as ligand. To our knowledge, this is the first reported detection of domoic acid, a causative agent of amnesic shellfish poisoning, in Japanese mussels.

scholarly journals Determination and Confirmation of the Amnesic Shellfish Poisoning Toxin, Domoic Acid, in Shellfish from Scotland by Liquid Chromatography and Mass Spectrometry

2001 ◽  
Vol 84 (5) ◽  
pp. 1657-1667 ◽  
Author(s):  
Philipp Hess ◽  
Susan Gallacher ◽  
Lesley A Bates ◽  
Nigel Brown ◽  
Michael A Quilliam
Keyword(s):  
Liquid Chromatography ◽  
Domoic Acid ◽  
Pecten Maximus ◽  
Shellfish Poisoning ◽  
Mussel Tissue ◽  
Crude Extracts ◽  
Amnesic Shellfish Poisoning ◽  
Routine Monitoring ◽  
Strong Anion Exchange ◽  
Array Detection

Abstract During 1998 and early 1999, shellfish samples from sites in Scotland were found to contain the amnesic shellfish poisoning toxin, domoic acid (DA). Two different techniques, liquid chromatography (LC) with UV diode-array detection and LC with mass spectrometric (MS) detection, were used to detect and confirm DA in shellfish extracts. The LC/UV method was validated for routine monitoring by recovery experiments on spiked mussel and scallop tissues with a certified mussel tissue used as reference material. Crude extracts of selected samples as well as extracts cleaned with strong anion exchange (SAX) were analyzed by both LC/UV and LC/MS. Good correlation (linear regression r2 = 0.996, slope = 0.93) between the 2 methods was found for cleaned extracts. Analyses of crude extracts by LC/UV produced false-positive results in 2 crab samples, whereas LC/MS analyses gave accurate results. It was concluded that LC/UV is a valid approach for routine monitoring of DA in shellfish when cleanup is performed with a SAX cartridge to prevent false positives. A variety of shellfish species were surveyed for DA content, including Pecten maximus (king scallops), Chlamys opercularis (queen scallop), Mytilus edulis (blue mussels), Cancer pugaris (crab), and Ensis ensis (razor fish). The highest concentration of DA was 105 μg/g in Pecten maximus.

scholarly journals Fast and Sensitive Method for Determination of Domoic Acid in Mussel Tissue

2016 ◽  
Vol 2016 ◽  
pp. 1-6 ◽  
Author(s):  
Elena Barbaro ◽  
Roberta Zangrando ◽  
Carlo Barbante ◽  
Andrea Gambaro
Keyword(s):  
Analytical Method ◽  
Domoic Acid ◽  
Shellfish Poisoning ◽  
Method Detection Limit ◽  
Mussel Tissue ◽  
Qualitative And Quantitative ◽  
Amnesic Shellfish Poisoning ◽  
The Matrix ◽  
Procedural Method

Domoic acid (DA), a neurotoxic amino acid produced by diatoms, is the main cause of amnesic shellfish poisoning (ASP). In this work, we propose a very simple and fast analytical method to determine DA in mussel tissue. The method consists of two consecutive extractions and requires no purification steps, due to a reduction of the extraction of the interfering species and the application of very sensitive and selective HILIC-MS/MS method. The procedural method was validated through the estimation of trueness, extract yield, precision, detection, and quantification limits of analytical method. The sample preparation was also evaluated through qualitative and quantitative evaluations of the matrix effect. These evaluations were conducted both on the DA-free matrix spiked with known DA concentration and on the reference certified material (RCM). We developed a very selective LC-MS/MS method with a very low value of method detection limit (9 ng g−1) without cleanup steps.

Sign in / Sign up

Export Citation Format

Share Document