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基于固定化金属亲和整体柱的痕量微囊藻毒素富集分析

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基于固定化金属亲和色谱(IMAC)识别原理,采用后修饰法在热引发自由基聚合反应得到的有机基质整体柱上直接固定Cu2+,设计并合成表征了poly(VIM-co-DVB)-Cu2+亲和毛细管整体柱,用于微囊藻毒素(MCs)的富集研究。详细优化了亲和整体柱的萃取条件,在最优条件下,将poly(VIM-co-DVB)-Cu2+整体柱用于毛细管微萃取(CME),并与高效液相色谱-质谱(HPLC-MS)检测技术联用,建立了环境水样品中3种MCs的高效富集分析方法。方法检出限为0。89~1。23ng/L,加标回收率为80。0%~105%,相对标准偏差(RSD)不大于6。8%。该方法灵敏度高、准确性好,可为污染水体中微囊藻毒素的监测分析提供有效手段。
Enrichment and Analysis of Trace Microcystins Based on Immobilized Metal Affinity Monolithic Column
The immobilized metal ion affinity chromatography(IMAC)theory was employed to design and synthesize a poly(VIM-co-DVB)-Cu2+monolithic column.The poly(VIM-co-DVB)matrix monolithic column was initially prepared via thermally initiated polymerization of 1-vinylimidazole(VIM)and divinylbenzene(DVB),and Cu2+was immobilized directly on the matrix monolithic col-umn through a post-modification multi-step method.The extraction conditions of the affinity monolith-ic columns were optimized.Under the optimal conditions,the poly(VIM-co-DVB)-Cu2+monolithic column was applied for capillary microextraction(CME)of microcystins(MCs)prior to high perfor-mance liquid chromatography-mass spectrometry(HPLC-MS)analysis in both tap water and lake wa-ter samples.The detection limits of MCs ranged from 0.89 to 1.23 ng/L,with recoveries between 80.0%and 105%,and the relative standard deviations(RSDs)were not more than 6.8%.The vali-dated CME/HPLC-MS methodology exhibits exceptional sensitivity and accuracy,making it a valu-able tool for the monitoring and analysis of MCs in environmental waters.

microcystins(MCs)immobilized metal affinity monolithic columnscapillary micro-extraction(CME)high performance liquid chromatography-mass spectrometry(HPLC-MS)

陈小燕、杨玲、苏立燊、吴晓苹

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福州大学 化学学院,食品安全与生物分析教育部重点实验室,福建 福州 350116

泉州市晋江环境监测站,福建 泉州 362200

福建省妇幼保健院,福建 福州 350001

微囊藻毒素 固定化金属亲和整体柱 毛细管微萃取 高效液相色谱-质谱

2025

分析测试学报
中国广州分析测试中心,中国分析测试协会

分析测试学报

北大核心
影响因子:1.498
ISSN:1004-4957
年,卷(期):2025.44(1)