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目的:建立水中痕量微囊藻毒素-RR、YR、LR、LW及LF的高效液相色谱-二极管阵列检测方法。方法:微囊藻毒素经C18固相萃取柱净化与浓缩,HPLC分离,二极管阵列检测,基质匹配和光谱图定性,外标法定量。结果:5种微囊藻毒素在0.1μg/ml~2.5μg/ml范围内具有良好的线性关系,检出限2.9 ng/L~3.6 ng/L,定量限9.5 ng/L~12 ng/L。三个浓度水平(0.2μg/L、1μg/L、2μg/L)的平均加标回收率56%~105%,RSD 2.2%~6.0%。重复取样测量日内RSD≤2.8%,日间RSD≤3.6%。结论:该方法采用多重定性,增强了水中痕量微囊藻毒素定性的准确性,检测限低,回收率高,可应用于水中微囊藻毒素的测定。
OBJECTIVE: To establish a high performance liquid chromatography-diode array detection method for trace microcystin-LR, YR, LR, LW and LF in water. Methods: The microcystin was purified and concentrated by C18 solid phase extraction (SPE) column, HPLC separation, diode array detection, matrix matching and spectroscopy qualitative analysis and external standard method. Results: The five microcystins showed good linearity in the range of 0.1μg / ml ~ 2.5μg / ml with the detection limit of 2.9 ng / L ~ 3.6 ng / L and the limit of quantification of 9.5 ng / L ~ 12 ng / L . The average recoveries were 56% -105% and RSD 2.2% -6.0% at three concentration levels (0.2μg / L, 1μg / L, 2μg / L). Repeated sampling measurement RSD ≤ 2.8% day RSD ≤ 3.6%. Conclusion: The method is multi-qualitative, which enhances the qualitative determination of trace microcystin in water with low detection limit and high recovery rate. It can be applied to the determination of microcystin in water.