Detection Technology of Microcystins in Aquatic Product by HPLC
Jinnan Wu
Abstract
Jinnan Wu
Abstract
To optimize the solid-phase extraction method of isolation, purification and determination of intracellular Microcystin-RR, -LR ( MC-RR,-LR ) , the sample was a black big head carp which enriched Microcystins. A method for trace level analysis of Microcystins in aquatic product using SPE and HPLC was developed, and the aquatic product was detected by diode array detection ( LC-DAD ) at 238 nm. During extraction, samples which enriched Microcystins were treated with different solvent ( 5 % acetic acid, 75 % methanol and mixed solvents 1-butanol,methanol,and water ( 1 ∶ 4 ∶ 15 ) ,eluted with 80 % methanol. Further, gradient elution was employed to separate microcystins in high performance liquid chromatography ( HPLC ) , the mobile phase consisted of 55 % methanol with small amount of trifluoroacetate acid ( TFA ) .The recoveries of MC-RR and MC-LR were 84.1 % and 89.9 % ,respectively. And the linear range is from 0.25 to 5g/L.The method is simple, sensitive, stable and suitable for the determination of the two most common Microcystins -LR,-RR.
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To optimize the solid-phase extraction method of isolation, purification and determination of intracellular Microcystin-RR, -LR ( MC-RR,-LR ) , the sample was a black big head carp which enriched Microcystins. A method for trace level analysis of Microcystins in aquatic product using SPE and HPLC was developed, and the aquatic product was detected by diode array detection ( LC-DAD ) at 238 nm. During extraction, samples which enriched Microcystins were treated with different solvent ( 5 % acetic acid, 75 % methanol and mixed solvents 1-butanol,methanol,and water ( 1 ∶ 4 ∶ 15 ) ,eluted with 80 % methanol. Further, gradient elution was employed to separate microcystins in high performance liquid chromatography ( HPLC ) , the mobile phase consisted of 55 % methanol with small amount of trifluoroacetate acid ( TFA ) .The recoveries of MC-RR and MC-LR were 84.1 % and 89.9 % ,respectively. And the linear range is from 0.25 to 5g/L.The method is simple, sensitive, stable and suitable for the determination of the two most common Microcystins -LR,-RR.
Key concepts: Chromatography, High-performance liquid chromatography, Chemistry, Methanol, Elution, Chromatography detector, Extraction (chemistry), Solid phase extraction