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多残留超高效液相色谱-高分辨质谱法分析饮用水中 21 种微囊藻毒素。

Multi-residue Ultra Performance Liquid Chromatography-High resolution mass spectrometric method for the analysis of 21 cyanotoxins in surface water for human consumption.

机构信息

Italian National Health Institute, Department of Environment and Health - Section of Water and Health, Viale Regina Elena, 299, 00161, Rome, Italy; University of Rome "Sapienza", Department of Pharmaceutical Science, Piazzale Aldo Moro, 5, 00161, Rome, Italy.

University of Rome "Sapienza", Department of Pharmaceutical Science, Piazzale Aldo Moro, 5, 00161, Rome, Italy.

出版信息

Talanta. 2020 May 1;211:120738. doi: 10.1016/j.talanta.2020.120738. Epub 2020 Jan 14.

DOI:10.1016/j.talanta.2020.120738
PMID:32070620
Abstract

The presence of cyanobacteria and their toxins in water used as drinking water or for recreational purposes may represent a risk for human health. This work describes the development of an advanced analytical method for simultaneous determination of 21 cyanotoxins (including Microcystins, Cyanopeptolins, Anabaenopeptins and Microginins) in drinking water based on Ultra Performance Liquid Chromatography coupled with a Q-TOF mass spectrometer. Water samples, spiked with Nodularin as internal standard at 1 μg/L, were extracted using Carbograph 4 SPE cartridge and 10 μL of the extracted sample were injected into the UPLC-HRMS/MS system. Analytes separation was obtained using a UPLC C18 column, acetonitrile and water as mobile phases, both containing 10 mM formic acid, and operating in positive ionization mode and sensitivity mode. The method has been proven to be robust, precise and accurate with recovery percentages above 85% and with relative standard deviations ≤16% and LODs between 0.002 and 0.047 μg/L, fitting for the intended purposes at the concentrations of interest. This method was applied during a monitoring activity in an Italian volcanic lake in Viterbo (Lazio Region, Italy), due to a severe algal proliferation in January 2018-March 2019 period and for the assessment of cyanobacteria proliferation risk and of cyanotoxin production in drinking water chain.

摘要

水中存在蓝藻及其毒素,无论是用于饮用水还是娱乐用水,都可能对人类健康构成威胁。本工作开发了一种基于超高效液相色谱-四极杆飞行时间串联质谱联用仪的先进分析方法,用于同时测定饮用水中的 21 种(包括微囊藻毒素、环肽、鱼腥藻肽和麦角甾醇)蓝藻毒素。水样经 Carbograph 4 SPE 萃取小柱萃取,内标 Nodularin 浓度为 1μg/L,10μL 萃取液注入 UPLC-HRMS/MS 系统。采用 UPLC C18 柱,以乙腈和水为流动相,均含 10mM 甲酸,在正离子化模式和灵敏度模式下进行分析物分离。该方法具有良好的稳健性、精密度和准确性,回收率大于 85%,相对标准偏差≤16%,检出限为 0.002-0.047μg/L,适用于目标浓度下的监测活动。该方法应用于 2018 年 1 月至 2019 年 3 月意大利拉齐奥地区维泰博(Viterbo)一座火山湖的监测活动中,评估藻华风险和饮用水中蓝藻毒素的产生。

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