HPLC-高分辨飞行时间质谱测定水中多种微囊藻毒素

Determination of Microcystins in Water by HPLC-Quadrupole-High Resolution Time of Flight Mass Spectrometry

水样经HLB小柱富集、净化后,采用高效液相色谱-四极杆-高分辨飞行时间质谱同时测定水样中MC-LA、MC-LF、MC-LR、MC-LW、MC-LY、MC-RR、MC-YR、MC-WR等8种微囊藻毒素。试验表明,8种微囊藻毒素在0.500μg/L^100μg/L范围内线性良好,方法检出限为0.001μg/L^0.005μg/L,自来水空白样品3个质量浓度水平的加标回收率为72.5%~99.8%,5次测定结果的RSD为1.9%~11.2%。将该方法用于测定珠海本地水产养殖鱼塘和小型水库的水样,结果均未检出。

8 kinds of microcystin,MC-LA,MC-LF,MC-LR,MC-LW,MC-LY,MC-RR,MC-YR and MC-WR,in water were purified and enriched by HLB column and determined simultaneously by high performance liquid chromatography-quadrupole-high resolution time of flight mass spectrometry(HPLC-Q-TOF).The experimental results showed that the calibration curves of microcystins had good linearity in the range of 0.500μg/L to 100μg/L.The detection limits were between 0.001μg/L and 0.005μg/L.The recoveries of blank samples at three mass concentration levels were from 72.5%to 99.8%,the RSDs of five measurements were from 1.9%to 11.2%.The method was applied in monitoring the water samples from local aquaculture fishponds and small reservoirs in Zhuhai,the results of the 8 kinds of microcystin were not detected.