【摘要】 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。更多还原

【Abstract】 Objective To develop a method to determine trace microcystin-LR and microcystin-RR in drinking water by UHPLC-MS/MS after immunoaffinity purification. Methods After the purification by the immunoaffinity column with 50 ml water sample and 0.25 mg of ascorbic acid, the chromatography separation was performed on an XDB-C18 column by methanol and water(with 0.1% formic acid), as mobile phase, in gradient elution program. MS/MS was performed by electrospray ionization in positive mode with multiple reaction monitoring(MRM) mode. Results The microcystin-LR and microcystin-RR were in the good linear ranges of 0.20-10 ng/ml, and the limits were 0.002 ng/ml. The average recoveries were 90.5%-110.6%,and the relative standard deviations(RSDs) ranged from 5.5 % to 10.6 %. Conclusion This method is more rapid, sensitive,efficient, accurate and suitable for determination of microcystin in water.更多还原