固相萃取-高效液相色谱-二极管阵列检测器法同时测定湖水中10种蓝藻毒素

Simultaneous Determination of 10 Kinds of Cyanotoxins in Lake Water by Solid Phase Extraction-High Performance Liquid Chromatography Coupled with Photodiode Array Detector

建立了固相萃取-高效液相色谱-二极管阵列检测器法测定湖水中10种蓝藻毒素(MC-RR、MC-YR、MC-Hty R、MC-LR、MC-WR、MC-LA、MC-LY、MC-LW、MC-LF和NOD)的方法。水样经固相萃取净化后,用Waters PAH C_(18)(250 mm×4.6 mm,5μm)色谱柱,以乙腈和含0.05%三氟乙酸为流动相梯度洗脱,流速为0.8 m L/min,柱温为30℃,进样量为20μL,二极管阵列检测器检测范围190~300 nm,检测波长为238 nm。根据保留时间、二极管阵列检测器全扫描光谱和色谱峰纯度分析等进行定性分析。10种蓝藻毒素在0.05~2.00 mg/L浓度范围内线性关系良好,线性系数R为0.9998~0.9999,方法检出限为0.005~0.020μg/L。3个浓度加标水平(0.1、1.0和1.8 mg/L)的回收率为85.1%~105.3%,相对标准偏差为0.8%~9.2%。本方法适用范围广、操作简单、分析速度快、灵敏度高、重现性和回收率好,采用多重定性增强了定性分析的准确性,可用于实际湖水中10种蓝藻毒素的测定。

A method has been developed by solid phase extraction-high performance liquid chromatography coupled with photodiode array detector for simultaneous determination of10kinds of cyanotoxins in lake water,including microcystin-RR(MC-RR),MC-YR,MC-HtyR,MC-LR,MC-WR,MC-LA,MC-LY,MC-LW,MC-LF and nodularin(NOD).The samples were enriched and purified by a HLB solid phase extraction column.The separation was performed on a Waters C18column(250mm伊4.6mm,5um)with the gradient elution of acetonitrile and water containing0.05%trifluoroacetic acid.The flow rate of the mobile phase was0.8mL/min.The column temperature was30℃and the injection volume was20uL.The photodiode array detector was scanned from190nm to300nm and the detection wavelength was238nm.Multiple qualitative analyses were completed according to retention time,full scanning spectrum of photodiode array detector and purity analysis of chromatographic peak.Good linearity was observed in the cyanotoxin concentration range of0.05mg/L-2.0mg/L with correlation coefficients(R)from0.9998to0.9999.The limits of detection for10cyanotoxins were in the range of0.005ug/L-0.020ug/L.The recoveries were in the range of85.1%-105.3%at the three spiked levels of0.1mg/L,1.0mg/L and1.8mg/L with the relative standard deviations(RSD)of0.8%-9.2%.The method was characterized by wide applicability,convenient operation,quick analytical rate,high sensitivity,good accuracy and high recovery.The qualitative accuracy was improved by using multiple qualitative analyses.This method was successfully applied to determination of10kinds of cyanotoxins in lake water.