超高效液相色谱-串联质谱分析蓝藻中微囊藻毒素的总量  

Determination of total cyanobacterial hepatotoxins microcystins in Tai Lake by the ultra performance liquid chromatography-mass chromatography

作　　者：徐夏叶 虞锐鹏[2] 陶冠军[2] 王利平[2] 张爽[2] 陈海燕[3] 宋启军 

机构地区：[1]江南大学化学与材料工程学院,无锡214122 [2]江南大学食品科学与技术国家重点实验室,无锡214122 [3]浙江省宁波市鄞州区疾病预防控制中心,宁波315100

出　　处：《分析试验室》2013年第3期22-25,共4页Chinese Journal of Analysis Laboratory

基　　金：国家自然科学基金(21175060);江苏省大型科学仪器设备共享服务平台(BZ201104)资助

摘　　要：建立了超高效液相色谱-串联质谱对蓝藻中微囊藻毒素总量的测定方法。样品采用乙酸及甲醇溶液进行抽提后离心,上清液经浓缩用固相萃取柱进行富集、纯化,洗脱液经0.025 mol/L KMnO4和饱和NaIO4溶液在pH 9条件下氧化1h。以BEH C18色谱柱进行梯度洗脱分离,采用离子监测质荷比(m/z 131.10)定量分析。微囊藻毒素总量的回收率在82.0%～98.6%之间。微囊藻毒素总量的检出限为0.80μg/L。该方法适用于测定蓝藻中的微囊藻毒素总量分析。A method for ultra performance liquid and methanol. After cen the determination of total cyanobacterial hepatotoxins microcystins in Tai Lake by the chromatography-mass chromatography was proposed. Samples were extracted with HAc trifugation, the concentrate was enriched and purified by C18 SPE. Eluent was oxidized by 0. 025 mol/L KMnO4 and saturated NaIO4 solution for 1 hour at pH 9. Separation of targeted analytes was achieved by a gradient elution program on a BEH C18 column. The protonated molecule m/z 131.10 was selected in the selected ion monitoring mode for specific measurement. The recoveries for spiked samples were in the range of 82.0% - 98.6%. The limits of detection was as low as 0. 80 μg/L. The method was applicable to determining total cyanobacterial hepatotoxins microcystins in Tai Lake.

关 键 词：超高效液相色谱-串联质谱 微囊藻毒素总量 2-甲基-3-甲氧基4-苯基丁酸 

分 类 号：O657.63[理学—分析化学]