A method for rapid detection of microcystin in water
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A technology for microcystin and water detection, which can be applied to measurement devices, instruments, scientific instruments, etc., can solve problems such as insufficient sensitivity, and achieve the effect of improving sensitivity, good repeatability, and satisfying rapid analysis.
Active Publication Date: 2020-03-20
浙江中一检测研究院股份有限公司
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[0006] The technical problem to be solved by the present invention is to provide a method for rapid detection of microcystins in water by copper sulfide nanomaterial enrichment-high performance liquid chromatography-electrospray tandem mass spectrometry, using copper sulfide Nanomaterials enrich and purify algal toxins, and use high performance liquid chromatography-tandem mass spectrometry to analyze microcystin MC-LR and MC-RR, which solves the problem of direct detection of algal toxins by high performance liquid chromatography-tandem mass spectrometry. For the problem of insufficient sensitivity, the detection of algal toxins can be realized within 20 minutes, and it has the characteristics of high sensitivity, fast analysis speed, strong method selectivity, and simple operation.
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[0034] The preparation method of the above-mentioned copper sulfide nanomaterials, the specific steps include: adding 0.2 ~ 1.0g CuSO 4 ·5H 2 O and 0.2g~1.0g polyvinylpyrrolidone (PVC) were dissolved in deionized water, and 0.1~1.0 mol / L NaOH and 1~2ml CS were added dropwise under stirring 2 After 10 minutes, it was transferred to a hydrothermal reaction kettle, kept at 140°C for 18h, cooled to room temperature after hydrothermal reaction, washed with deionized water and ethanol, and dried in vacuum at 60°C for 6h.
[0035] Ammonia and formic acid are preferably used to adjust the pH value of the water sample in the above step 1.
[0036] The conditions of use of the liquid chromatographic instrument in the above step 2 are: the liquid chromatographic instrument used is the AcquityUPLC system, and the microcystin in the sample is separated through the Acquity UPLC BEH C18 chromatographic column. The chromatographic column: Acquity UPLC BEH C18, 1.7 μm, 2.1×100mm; column temp...
Embodiment 1
[0046] Preparation of copper sulfide nanomaterials:
[0047] 0.2gCuSO 4 ·5H 2 O and 0.2 g polyvinylpyrrolidone (PVC) were dissolved in deionized water, and 0.5 mol / L NaOH and 2 ml CS were added dropwise with stirring 2 After 10 minutes, it was transferred to a hydrothermal reaction kettle, kept at 140°C for 18h, cooled to room temperature after hydrothermal reaction, washed with deionized water and ethanol, and dried in vacuum at 60°C for 6h.
Embodiment 2
[0049] Enrichment of water samples:
[0050] After the water sample was filtered through a 0.2 μm polypropylene filter membrane, 8 mg of copper sulfide nanomaterials washed with methanol and pure water were added, vortexed and mixed, and then ultrasonicated for 2 minutes for enrichment and purification. Then the water body is quickly passed through the filter, and finally eluted with pure water and methanol.
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Abstract
The invention discloses a method for quickly detecting microcystins in water. The method comprises the following steps: 1, filtering an obtained water sample, enriching and purifying the water samplewith a transition metal sulfide nano-material, and quickly passing the water through a filter, adjusting pH of the water sample to 1-5, and finally performing elution with pure water and methanol; 2,analyzing and determining the treated water sample with ultra-high performance liquid chromatography-tandem mass spectrometry. After the water sample is enriched and purified by the transition metal sulfide nanomaterial, MC-LR and MC-RR sensitivity can reach 20 ng / L and 10 ng / L respectively through cooperation with the ultra-high performance liquid chromatography- tandem mass spectrometry, the whole process time is shorter than 20 min, and dual requirements of the environmental monitoring department for timeliness and accuracy of microcystin detection can be fully met. Standard addition experiments prove that the recovery range of drinking water samples with the method reaches 97%-105%, and the recovery rate for waste water samples reaches 83%-99%, and the relative standard deviation is smaller than 5%. The method has the characteristics of high sensitivity, high analysis speed, high selectivity, simple operation and the like.
Description
technical field [0001] The invention relates to a method for detecting microcystins in water, in particular to a method for rapidly detecting microcystins in water by copper sulfide nanometer material enrichment-high performance liquid chromatography-electrospray tandem mass spectrometry. Background technique [0002] Water blooms caused by eutrophication of water bodies have caused a lot of environmental problems in the past few decades, among which water bloom events such as Taihu Lake and Dianchi Lake have attracted widespread attention all over the world. During the algae bloom process, a large number of algae accumulate and emit toxic products—algal toxins, which pose a serious threat to various organisms in the environmental water body. Microcystins (Microcystins, MCs) are one of the most common types of cyanotoxins, and a variety of algae can produce microcystins. It is a group of single-ring heptapeptide substances, in which there are two variable amino acids. So fa...
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