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[目的]建立水中微囊藻毒素(MC)含量的高效液相色谱初筛、光谱定性、质谱确认分析方法。[方法]以Waters Atlantis dC18(3μ2.1×100 mm),色谱质谱柱为分析柱,流动相:20%甲醇溶液,Surveyor二极管阵列检测器(PDA)和Finnigan LCQ Deca XP MAX质谱仪为检测器。[结果]回归方程和相关系数为:MC-RR y=7.401998×1025 x+5.028972×102,r=0.998;MC-LR y=5.689824×105x+5.925834×102,r=0.9996;MC-YR y=4.816086×105x+6.145898×102,r=0.9994。平均回收率为=95.1%~105.0%,RSD为3.00%~4.99%。[结论]用HPLC-PDA法检测水源水中的微囊藻毒素方法简便,重现性好,灵敏度高,定性准确,定量精确。
[Objective] To establish a preliminary screening, spectrophotometric and mass spectrometric confirmation method for microcystin (MC) in water. [Method] With Waters Atlantis dC18 (3μ2.1 × 100 mm) and chromatographic column as the analytical column, the mobile phase was 20% methanol solution, Surveyor diode array detector (PDA) and Finnigan LCQ Deca XP MAX mass spectrometer . [Results] The regression equation and the correlation coefficient were: MC-RR y = 7.401998 × 1025 × + 5.028972 × 102, r = 0.998; MC-LR y = 5.689824 × 105x + 5.925834 × 102, r = 0.9996; MC-YR y = 4.816086 × 105x + 6.145898 × 102, r = 0.9994. The average recovery was 95.1% ~ 105.0%, RSD was 3.00% ~ 4.99%. [Conclusion] The method of HPLC-PDA for the determination of microcystins in drinking water was simple, reproducible, sensitive and accurate.