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Method for detecting microcystic toxins in water

A technology for microcystin and water detection, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of being easily disturbed by the surrounding environment, insufficient sensitivity, complicated steps, etc., and overcome the complicated and repetitive pretreatment steps Good, high-accuracy effect

Inactive Publication Date: 2021-11-16
CHINESE RES ACAD OF ENVIRONMENTAL SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the method of Zhang Ming et al. requires manual solid-phase extraction for sample pretreatment, the steps are complex and time-consuming, and the sample pretreatment process is easily disturbed by the surrounding environment; while the detection limit of Li Xiangang et al.’s method is as high as 0.01 ~0.6ug / L, sensitivity is not enough

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  • Method for detecting microcystic toxins in water
  • Method for detecting microcystic toxins in water
  • Method for detecting microcystic toxins in water

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] Simultaneous detection of eight microcystins in water samples by online solid-phase extraction ultra-performance liquid chromatography-tandem mass spectrometry (Online-SPE UPLC-MS / MS).

[0057] ①Preparation of standard stock solutions: Prepare 1.0 mg / L methanol single-standard stock solutions (MC-RR, MC-LR, MC-YR, MC-WR, MC-LA, MC-LF, MC-LY, MC- LW), stored at -20°C in the dark and pipetted. An appropriate amount of 8 kinds of microcystin standard substances is diluted with chromatographically pure methanol, and diluted with chromatographically pure methanol to the required mass concentration when used. Use chromatographically pure methanol to prepare an internal standard solution with a concentration of 50.0 μg / L leucine enkephalin, store it below -20°C for use, and dilute it with chromatographically pure methanol to the required mass concentration.

[0058] Eight kinds of microcystin single standard solutions were prepared with chromatographically pure methanol to pr...

Embodiment 2

[0071] ①Measure 24 ultrapure water samples of 20 ml each, 6 of which are used as sample blanks, and add microcystin mixed standard solution to the remaining 18 samples, and make 3 addition levels respectively. After adding 8 kinds of Microcystis The total concentrations of the toxins were 50ng / L, 100ng / L, and 500ng / L, and each addition level was measured in parallel 6 times; among them, the microcystin mixed standard solution was a mixed standard solution containing 8 kinds of MCs at the same time. When preparing, Prepare 1.0 mg / L methanol single standard stock solution (MC-RR, MC-LR, MC-YR, MC-WR, MC-LA, MC-LF, MC-LY, MC-LW), and store at -20°C Light preservation pipetting. Take 100 μL of each single-standard stock solution of 1.0 mg / L and 200 μL of methanol and mix evenly to obtain a mixed standard solution of 100 μg / L. The remaining concentrations of 50 ng / L, 100 ng / L, and 500 ng / L are diluted to Need mass concentration to get.

[0072] ② Filter through a 0.22 μm MCE filt...

Embodiment 3

[0080] Embodiment 3 is basically the same as Embodiment 1, the difference is:

[0081] In the pretreatment of water samples, three groups of experiments were carried out using three kinds of filter membranes, and the other experimental conditions of each group of experiments were the same as in Example 1; the three kinds of filter membranes were respectively 0.22 μm polyethersulfone filter membrane (PES filter Membrane), 0.22 μm polytetrafluoroethylene filter membrane (PTFE) filter membrane, 0.22 μm mixed cellulose ester filter membrane (MCE filter membrane).

[0082] The recovery rate of 8 kinds of microcystins under the use situation of 3 kinds of different filter membranes of present embodiment, as figure 2 As shown, the chromatograms of 8 microcystins under the use of 3 different membranes, such as image 3 shown.

[0083] From figure 2 It can be seen that under the use of MCE membrane, the recovery rate of 8 kinds of MCs ranges from 79-108%, which meets the standard ...

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Abstract

The invention relates to a method for detecting microcystic toxins in water, which comprises the following steps: filtering a water sample through a 0.22 mu m MCE filter membrane, and then carrying out on-line solid-phase extraction and analytical determination on the filtered water sample through an on-line solid-phase extraction ultra-high performance liquid chromatography-tandem mass spectrometry method, wherein the online solid-phase extraction adopts a C8 solid-phase extraction column, the conditions of the ultra-high performance liquid chromatography are as follows: in a mobile phase, a solution A is a 0.1% formic acid acetonitrile solution, and a solution B is a 0.1% formic acid aqueous solution; the gradient elution procedure includes that in 0-4.6 min, and 98% of the solution B is used; in 4.6-10.0 min, 98% liquid B and 25% liquid B are used, and in 10.0-11.0 min, 25% liquid B and 100% liquid B are used; the flow rate is 0.4 mL / min; the column temperature is 35 DEG C, and the sample injection volume is 2mL. The method disclosed by the invention is a method which is high in sensitivity, high in accuracy, good in recovery rate and reproducibility, simple, convenient and rapid to operate and capable of simultaneously determining the eight MCs in the water body.

Description

technical field [0001] The invention belongs to the technical field of water environment monitoring, and relates to a method for detecting microcystins in water, in particular to a method for detecting microcystins in water by an online solid-phase extraction ultra-high performance liquid chromatography tandem mass spectrometry. Background technique [0002] With the development of industrial and agricultural production, a large amount of nitrogen and phosphorus are discharged into water bodies, resulting in increasingly serious eutrophication of water bodies. The eutrophication of water bodies will lead to the appearance of cyanobacteria blooms, and cyanobacteria blooms can release secondary metabolites of biotoxins, such as microcystins (Microcystins, MCs), etc., causing pollution of various derivatives and endangering humans and other organisms. safety. Epidemiological studies have found that the high incidence of primary liver cancer in some areas in southern my country...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/14G01N30/34G01N30/36G01N30/60G01N30/72
Inventor 刘琰葛思敏乔肖翠李雪赵兴茹刘承友齐童焦立新储昭升丁帅
Owner CHINESE RES ACAD OF ENVIRONMENTAL SCI
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