EPA-OW: BreveLCMS: Brevetoxin in water by LCMS
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Official Method Name
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LC/MS analysis of brevetoxin metabolites in the Eastern oyster |
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Current Revision
| 2004 |
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Media
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WATER |
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Instrumentation
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Liquid Chromatography-Mass Spectrometery (also High Performance LC-MS; HPLC-MS) |
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Method Subcategory
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Biotoxin |
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Method Source
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Citation
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Wang Z, Plakas SM, El Said KR, Jester EL, Granade HR, Dickey RW., 2004, LC/MS analysis of brevetoxin metabolites in the Eastern oyster (Crassostrea virginica): Toxicon. 2004. 43(4): 455 - 465. |
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Brief Method Summary
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Shellfish sample homogenates are extracted with acetone, and centrifuged. The supernatants are combined, evaporated, and re-solubilized in 80% methanol. Following a wash with 95% n-hexane, the methanolic layer is evaporated, and the residue re-solubilized in 25% methanol and applied to a C18 SPE column. Analytes are eluted with 100% methanol, evaporated, and re-solubized in methanol for analysis. Analysis of prepared samples is performed using HPLC-MS-MS with a mobile phase of water and acetonitrile with acetic acid. Analytes are detected by an MS with ESI interface. Brevetoxins are extensively metabolized, with many sub-forms. This method describes multiple liquid chromatography/electrospray ionization mass spectrometry (LC-ESI-MS) profiles for metabolites of brevetoxins from oysters. |
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Scope and Application
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This method is for extracting and detecting Brevetoxins in shellfish and can be used for water. Because it has not been validated for use in water, it is listed as a screening method. |
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Applicable Concentration Range
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Interferences
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May have extraction interfences by non-target compounds. |
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Quality Control Requirements
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SAM lists these procedures for detection in solid, particulate, aerosol, liquid, and water samples. Further research is needed to develop and standardize the procedures for environmental sample types. |
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Sample Handling
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Maximum Holding Time
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Relative Cost
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Less than $50 |
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Sample Preparation Methods
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