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目的建立免疫亲和柱-高效液相色谱-串联四极杆质谱测定饮用水中微囊藻毒素-LR和-RR的方法。方法取50 ml水样加0.25 mg抗坏血酸后,经免疫亲和柱净化,XDB-C18色谱柱分离,以乙腈-0.1%甲酸水溶液为流动相进行梯度洗脱;采用电喷雾离子源,以多反应监测(MRM)方式正离子化模式进行检测。结果微囊藻毒素-LR和微囊藻毒素-RR在0.20~10 ng/ml范围内线性良好,方法检出限为0.002 ng/ml。该方法平均加标回收率为90.5%~110.6%,相对标准偏差为5.5%~10.6%。结论该方法灵敏度高,操作简便、分析时间短,可更好地满足饮用水监测的需要。
Objective To establish a method for the determination of microcystin-LR and -RR in drinking water by immunoaffinity column-high performance liquid chromatography-tandem quadrupole mass spectrometry. Methods 50 ml of water sample plus 0.25 mg of ascorbic acid was purified by immunoaffinity column and separated by XDB-C18 column with gradient elution with acetonitrile-0.1% formic acid as mobile phase. Electrospray ionization Monitoring (MRM) mode positive ionization mode for testing. Results microcystin-LR and microcystin-RR ranged from 0.20 ng / ml to 10 ng / ml. The detection limit was 0.002 ng / ml. The average recoveries of this method ranged from 90.5% to 110.6% with relative standard deviations of 5.5% -10.6%. Conclusion The method has high sensitivity, easy operation and short analysis time, which can better meet the needs of drinking water monitoring.