超高效液相色谱-四极杆-飞行时间质谱法快速测定蓝藻水华堆积处理池中四种微囊藻毒素
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摘要
通过有机溶剂高速匀浆、固相萃取纯化、超高效液相色谱-四极杆-飞行时间质谱(UPLC-Q-TOF-MS)联用技术快速测定蓝藻水华堆积处理池的微囊藻毒素-RR、-YR、-LR和-WR等四种藻毒素。分别采用选择离子监测质荷比(m/z)为519.81、1045.58、995.64、1068.61分子离子峰进行定量分析。该法检出限为1.0-5.0μg/kg,在浓度0.01-1.0 mg/kg的范围内,峰面积与样品浓度呈良好线性关系;4种藻毒素的回收率为83.0-96.1%,相对标准偏差为4.6-12.6%。采用上述方法对太湖蓝藻各藻水分离站堆积处理池中蓝藻进行测定,其中微囊藻毒素-RR最高含量为0.082 mg/kg,微囊藻毒素-LR最高含量为0.047 mg/kg。此方法快速、准确、灵敏度高、专属性好,为有效评价蓝藻水华脱毒处理效果提供依据。
In this paper, a new analytical method, based on Organic solvent extraction and solid phase extraction, the ultra performance liquid chromatography-quadrupole-time of flight mass spectrometry(UPLC-Q-TOF-MS) was developed for the determination of four microcystins from sedimentation ponds for the treatment of Cyanobacterial Blooms. The protonated molecule was selected in the selected ion monitoring m/z 519.84, 1045.66, 995.67, 1068.61 for specific measurement of microcystin(MC) variant-RR,-YR,-LR and-WR. The limits of detection as low as 1.0-5.0μg/kg with linear range between 0.01-1.0mg/kg were achieved for four cyanotoxins. The recoveries for spiked samples were in the range of 83.0-96.1% with RSD between 4.6-12.6%. The concentration of MC-RR, MC-LR observed are as high as 0.082, 0.047 mg/kg dry weight, the contents of microcystins in sedimentation ponds. The method is highly selective and sensitive for measurements of MCs and is adequate for analysis of MCs in these treatment ponds.
引文
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