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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 the determination of microcystin in cyanobacteria by ultra performance liquid chromatography-tandem mass spectrometry was established. The sample was extracted with acetic acid and methanol and centrifuged. The supernatant was concentrated and purified by solid-phase extraction. The eluate was oxidized by 0.025 mol / L KMnO4 and saturated NaIO4 solution for 1 h at pH 9. Gradient elution was performed on a BEH C18 column and quantified by ion monitoring mass-to-charge ratio (m / z 131.10). The recovery rates of total microcystin were between 82.0% and 98.6%. The detection limit of total microcystin was 0.80μg / L. The method is suitable for the determination of total microcystins in cyanobacteria.