直接进样-超高效液相色谱-三重四极杆质谱法同时快速测定水中12种微囊藻毒素和1种节球藻毒素

建立了超高效液相色谱-三重四极杆质谱快速检测水中12种微囊藻毒素(MCs)和1种节球藻毒素(NOD)的分析方法。水样经甲醇等体积稀释,聚醚砜(PES)滤膜过滤,滤液直接进样分析,以0.1%(v/v)甲酸乙腈溶液和0.2%(v/v)甲酸水溶液作为流动相进行梯度洗脱,采用ACQUITY UPLC BEH 300 C18柱(100 mm×2.1 mm,1.7μm)进行分离,在电喷雾正离子模式下以MRM方式进行检测,标准溶液外标法定量。方法的检出限为0.03~0.1μg/L,定量限为0.1~0.3μg/L。对自来水和河水样品进行加标回收试验,目标物的平均加标回收率为79.5%~123%,相对标准偏差为1.0%~20%(n=6)。该法简单、灵敏、准确,适用于水中12种微囊藻毒素和1种节球藻毒素的快速测定。

Simultaneous rapid determination of 12 microcystins and one nodularin in water by direct injection-ultra performance liquid chromatography-triple quadrupole mass spectrometry

A rapid method was developed for the simultaneous determination of 12 microcystins (MCs) and one nodularin (NOD) in water by direct injection-ultra performance liquid chromatography-triple quadrupole mass spectrometry (UPLC-MS/MS). The water samples were first diluted with equal volume of methanol, and then filtered through polyether sulfone (PES) syringe filter. The filtrates were directly injected into the UPLC system. The separation of the analytes was carried out on an ACQUITY UPLC BEH 300 C₁₈ column (100 mm×2.1 mm, 1.7 μm) with gradient elution using mobile phases of acetonitrile containing 0.1% (v/v) formic acid and 0.2% (v/v) formic acid aqueous solution. The 12 microcystins and one nodularin were detected by positive electrospray ionization in the multiple reaction monitoring (MRM) mode, and quantified by standard solvent external standard method. The limits of detection were 0.03-0.1 μg/L and the limits of quantification were 0.1-0.3 μg/L. The recoveries were in the range of 79.5%-123% with the relative standard deviations ranging from 1.0% to 20% (n=6). The method is simple, sensitive and accurate, and has been successfully applied to the detection of the 13 kinds of algae toxins in water.