在线固相萃取–液相色谱法测定水中3种微囊藻毒素

建立了在线固相萃取–液相色谱法测定水中3种微囊藻毒素的方法。采用Acclaim PA Cartridge在线固相萃取小柱(10 mm×4.3 mm,5μm),以KH2PO4缓冲溶液–甲醇为富集流动相,进样体积为10 m L。以KH2PO4缓冲溶液–乙腈为洗脱流动相,采用二极管阵列检测器进行检测,检测波长为238 nm。微囊藻毒素MC–LR,MC–RR在0.1~10.0μg/L范围内线性关系良好,MC–YR线性范围则为0.1~5.0μg/L,相关系数r2不小于0.998,3种微囊藻毒素MC–LR,MC–RR,MC–YR的检出限均为0.1μg/L(S/N=3),水源水加标回收率为96.9%~105.4%,测定结果的相对标准偏差为3.55%~6.46%(n=12)。该方法适用于水源水及饮用水中3种微囊藻毒素的快速测定。

Determination of Three Microcystins in Water by Online-SPE and HPLC

Three microcystins were determined by using online-solid phase extraction and high performance liquid chromatograpgy（HPLC）. Acclaim PA Cartridge（10 mm ×4.3 mm, 5 μm） was employed as online SPE, KH2PO4 buffer solution-methanol as enriched mobile phase. The injection volume was 10 mL. KH2PO4 buffer solution-acetonitrile was elution mobile phase. The detector was DAD at 238 nm. It had a good linear relation in the range of 0.1-10.0 μg/L （MC-YR was 0.1-5.0 μ g/L） with the correlation coefficients not less than 0.998. The limits of the three microcystins was 0.1 нg/L（S/N=3）. The recoveries of the method were 96.9%-105.4% with a good relative standard deviations of 3.55%- 6.46%（n=12）. This method is suitable for determination of three microcystins in surface water and drinking water fastly.