标准摘要
[中文适用范围]： 本文件规定了 12 种微囊藻毒素变体（微囊藻毒素-LR、-LA、-YR、-RR、-LY、-WR、-HtyR、-HilR、-LW、-LF、[Dha7]-微囊藻毒素-）的定量方法。 饮用水和淡水样品中的 LR 和 [Dha7]-微囊藻毒素-RR）浓度在 0.05 µg/l 至 1.6 µg/l 之间。 该方法可用于进一步测定微囊藻毒素，前提是每种微囊藻毒素的色谱和质谱检测的分析条件已经过测试和验证。 使用内标校准通过 LC-MS/MS 分析样品。 该方法是基于性能的。 允许实验室修改该方法，例如增加低干扰样品的直接流动注射体积或稀释样品以增加工作范围上限，前提是满足该方法中的所有性能标准。 附件 A 描述了通过高分辨率质谱 (HRMS) 检测微囊藻毒素作为串联质谱 (MS/MS) 的替代方法。 基于在线固相萃取与液相色谱联用的替代自动化样品制备方法描述于附录 B. 当仪器灵敏度不足以达到直接流动注射的方法检测限时，附录 C 中描述了固相萃取净化和浓缩步骤。 [外文原描述]： This document specifies a method for the quantification of twelve microcystin variants (microcystin-LR, -LA, -YR, -RR, -LY, -WR, -HtyR, -HilR, -LW, -LF, [Dha 7 ]-microcystin-LR, and [Dha 7 ]-microcystin-RR) in drinking water and freshwater samples between 0,05 µg/l to 1,6 µg/l. The method can be used to determine further microcystins, provided that analytical conditions for chromatography and mass spectrometric detection has been tested and validated for each microcystin. Samples are analysed by LC-MS/MS using internal standard calibration. This method is performance based. The laboratory is permitted to modify the method, e.g. increasing direct flow injection volume for low interference samples or diluting the samples to increase the upper working range limit, provided that all performance criteria in this method are met. Detection of microcystins by high resolution mass spectrometry (HRMS) as an alternative for tandem mass spectrometry (MS/MS) is described in Annex A. An alternative automated sample preparation method based on on-line solid phase extraction coupled to liquid chromatography is described in Annex B. When instrumental sensitivity is not sufficient to reach the method detection limits by direct flow injection, a solid phase extraction clean-up and concentration step is described in Annex C.
英文名称Water quality — Determination of microcystins — Method using liquid chromatography and tandem mass spectrometry (LC-MS/MS)