高效液相色谱-二极管阵列检测器测定水中5种微囊藻毒素

Determination of five microcystins in water by high performance liquid chromatography-photodiode array detector

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 method for determination of trace amounts of five microcystins （MCs） in water by using high performance liquid chromatography （HPLC） - photodiode array （PDA） detector. Methods： The five MCs in water were purified and concentrated by C18 solid phase extraction column, separated by HPLC, qualitatively analyzed by both matrix matching and spectrum charts, and quantitatively analyzed by external standard method. Results ： The five MCs showed a good linear relationship in the range of 0.1 μg/ml - 2.5 μg/ml, with the detection limit of 2.9 ng/L - 3.6 ng/L and quantitation limit of 9.5 ng/L - 12ng/L. The average recoveries of three spiked levels （0.2 p,g/L, 1 μg/L, 2μg/L） were 56% - 105% with the relative standard deviations （RSD） of 2.2% - 6.0%. RSD of intra - day and inter - day was less than 2.8% and 3.6% respectively. Conclusion ： This method can improve the accuracy of trace analysis of five MCs in water by using multiple qualitative analysis, applied to the detection of microcystins in water.