全自动固相萃取-高效液相色谱法同时测定饮用水中3种微囊藻毒素
Determination of three microcystins in drinking water by automatic- SPE and HPLC
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摘要: 建立全自动固相萃取-高效液相色谱法同时测定饮用水中3种微囊藻毒素的方法。采用全自动固相萃取仪代替传统的前处理方式,对大体积水样进行富集,以KH2PO4(p H=3.0)-甲醇(43∶57,v∶v)为流动相,采用二极管阵列检测器进行检测,结果 3种微囊藻毒素在0.110.0μg/m L范围内线性关系良好,相关系数r2≥0.999,3种不同微囊藻毒素的检出限均可达到0.05μg/L(S/N=3),加标回收率在86.3%99.7%范围内,标准偏差为1.70%2.72%(n=6),该方法用于测定饮用水中3种微囊藻毒素具有操作简单、快速,精密度高、准确可靠等特点。Abstract: Three microcystins were determined by automatic solid phase extraction( SPE) and high performance liquid chromatography( HPLC) in this study.Instead of the traditional pretreatment methods,Reeko automatic- SPE system was used for a fast enrichment process. Samples were chromatographed isocratically using a KH2PO4( p H3.0) buffer solution- methanol mobile phase on a C18 column in- line by diode array detector. Good linear relation were presented in the range of 0.1 ~ 10.0 μg / m L for all microcystins with the correlation coefficients R2≥0.999.The detection limits of three microcystins were 0.05 μg / L( S / N = 3).Recoveries of these microcystins at three different concentration levels were studied.The recoveries of this method were 86.3% ~99.7% with a good relative standard deviations of 1.70% ~ 2.72%( n = 6). This method was easy,fast and accurate and suitable for a rapid determination of microcystins in drinking water.