高效液相色谱法同时测定水源水中三种微囊藻毒素

目的 建立一种同时测定水源水中三种微囊藻毒素（MC-LR、MC-RR、MC-YR）的高效液相色谱（high performance liquid chromatography，HPLC）方法。 方法 取500 mL水样，0.45 μm滤膜过滤，滤液过C18柱，依次用10 mL超纯水、20 mL 20%甲醇溶液淋洗，15 mL 80% 甲醇溶液（加入0.05%三氟乙酸）洗脱，蒸发浓缩吹干，溶于1 mL超纯水，待测。采用固相萃取柱，流动相为0.1%磷酸水溶液-乙腈（67∶33），流速1.0  mL/min，柱温45℃，在238 nm波长紫外线检测器检测。结果 MC-LR、MC-RR和MC-YR 在 0.05~1.00 μg/mL范围内线性良好（r=0.9987、0.9992和0.9997），且峰形较好；回收率均在80%~110%，相对标准偏差（relative standard deviation，RSD）为5.0%~9.6%；MC-LR、MC-RR和MC-YR的方法检出限（limit of detection，LOD）分别为0.028 μg/L、0.037 μg/L和0.056 μg/L。结论 本方法准确度、灵敏度、回收率高，重现性好，可用于水源水中MC-LR、MC-RR、MC-YR同时检测。

Simultaneous determination of three microcystins in source water using high performance liquid chromatography

Objective A method was established for simultaneous determination of microcystins （microcystin-LR，-RR，-YR） in source water using high-performance liquid chromatography （HPLC）. Methods Water samples （500 mL） were filtered through a 0.45 μm membrane on a C18 column，then eluted with sequential use of 10 ml of ultra-pure water，20 mL of 20% methanol and 15 mL of 80% methanol containing 0.05% tallow fatty acid（TFA）. The eluate was dried and the residues were dissolved in 1 mL of ultra-pure water for testing. The eluate was fractionated on a C18  column with a mobile phase of 0.1% aqueous phosphoric acid-acetonitrile （67：33） at a flow rate of 1 ml/min at a column temperature of 45 ℃. Compounds were detected with a UV detector at a wavelength of 238 nm. Results Microcystin-LR，-RR，and -YR showed good peak shape and good linearity in the range of 0.05-1.0 μg/mL（r=0.9987， 0.9992，and 0.9997）. Recoveries ranged from 80% to 110%，relative standard deviation（RSD） was 5.0%-9.6%，and limits of detection were 0.028，0.037，and 0.056 μg/L. Conclusions The method described here can be used for accurate，highly sensitive，and reproducible simultaneous detection of microcystin-LR，-RR and -YR in source water.