高效液相色谱法测定蓝藻发酵液及堆肥中微囊藻毒素含量

Determination of Microcystins in Fermented Blue-green Algae Liquor and Blue-green Algae Compost by High Performance Liquid Chromatography

建立了高效液相色谱测定蓝藻发酵液和蓝藻堆肥中微囊藻毒素（MC-RR、MC-LR）含量的方法。样品中的MC-RR和MC-LR用5％乙酸溶液提取，离心分离后经过SPE小柱净化、富集，在C18柱上采用梯度洗脱，流动相为甲醇＋0．05mol／L磷酸二氢钾，利用二极管阵列检测器在238nm进行检测。MC-RR、MC-LR的检测限为0．03μg/ml，定量限为0．10μg/ml。在50-200μg/kg的添加范围内，MC-RR的回收率为78．0％-90．5％，MC-LR的回收率为82．0％-92．8％。

A method was developed for determination of microcystins （ MC-RR and MC-LR） in fermented blue-green algae liquor and blue-green algae compost by high performance liquid chromatography （HPLC）. The microcystins were extracted with 5% acetic acid and cleaned via a solid-phase extraction （SPE） cartridge. The analytes were separated on an ODS C18 column with methanol and 0. 05 mol/L KH2PO4 as the mobile phase in a gradient elution, and were detected by diode array detection （LC-DAD） at 238 nm. The limits of detection （LOD） and limits of quantification （LOQ） were 0. 03 μg/ml and 0. 10 μg/ml, respectively. The recoveries of MC-RR and MC-LR spiked at 50 - 200 μg/kg were 78. 0% - 90. 5% and 82.0% -92. 8%, respectively.