CN102608239A - Method and device for in-situ monitoring of microcystin - Google Patents

Method and device for in-situ monitoring of microcystin Download PDF

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Publication number
CN102608239A
CN102608239A CN2012100568453A CN201210056845A CN102608239A CN 102608239 A CN102608239 A CN 102608239A CN 2012100568453 A CN2012100568453 A CN 2012100568453A CN 201210056845 A CN201210056845 A CN 201210056845A CN 102608239 A CN102608239 A CN 102608239A
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microcystin
water
resin
analysis
monitoring
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CN102608239B (en
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李爱峰
赵慧
马菲菲
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Ocean University of China
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Ocean University of China
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Abstract

The invention relates to a method and a device for in-situ monitoring of microcystin, which utilize resin HP20 to absorb the microcystin in water. The method includes the detailed steps: firstly, placing a device filled with a resin bag into the water to absorb the microcystin; then eluting the microcystin with 75% methanol solution; and finally, utilizing a high performance liquid chromatography or liquid chromatography-mass spectrometry system for analysis. Real-time monitoring and early warning of the microcystin in potable water sources can be realized by means of in-situ acquisition of the microcystin and by combining desorption with high performance liquid chromatographic analysis. The method is simple in operation and low in cost, avoids biotransformation of toxin components, and the treated sample is pure in matrix so as to beneficial to qualitative and quantitative analysis of the chromatographic technique. Besides, compared with a traditional water sample analysis and biological monitoring method, the method is capable of detecting microcystin contamination in the water in advance, high in sensitivity and capable of realizing early warning of safety of water quality of the potable water sources.

Description

A kind of in-situ monitoring method of Microcystin and device thereof
Technical field
The invention belongs to little algae toxin monitoring technical field, be specifically related to a kind of in-situ monitoring method and device thereof of Microcystin, promptly utilize macroreticular resin original position absorption Microcystin, can monitor in real time and early warning Microcystin.
Background technology
Microcystin and human health are closely related, and report is arranged during, slow poisoning incident acute by the caused mankind of Microcystis aeruginosa poison rope.Microcystis aeruginosa poison rope mainly acts on liver cell and Kupffer cell, induces in the Kupffer cell generation from cytokine I, the activity of phosphoprotein phosphatase in the strong inhibition liver cell, and toxic action mainly shows as hepatotoxicity, promotes the generation of tumour.Microcystis aeruginosa also has certain toxicity to animal, after domestic animal and wild animal have been drunk the water that contains Microcystin, symptoms such as diarrhoea, weak, apocleisis, vomiting can occur, even dead.
At present, mainly be to gather water sample for the monitoring method of Microcystin through fixed point, with water sample concentrate with purification process after, through monitoring methods such as biology, physics and chemistry Microcystin is carried out qualitative and quantitative analysis, thereby reaches the purpose of monitoring.But this traditional monitoring technology specific aim is not strong, do not have the continuity in time and space, and the step of sample preparation is more loaded down with trivial details, is difficult to realize the early warning to the pollution of potable water seedbed Microcystin.
Summary of the invention
The in-situ monitoring method and the device thereof that the purpose of this invention is to provide a kind of Microcystin; It is a kind of method that can effectively monitor to the Microcystin in the water source; The device of Microcystin in a kind of adsorbed water body easily is provided simultaneously, thereby remedies the deficiency of prior art.
To the problem that the traditional monitoring of Microcystin technology exists, the applicant finds efficiently Microcystin in the adsorbed water body of macropore polymer resin in long term studies, thereby has facilitated the present invention.
Monitoring method of the present invention is to come the Microcystin in the adsorbed water body with the HP20 resin.
Monitoring method of the present invention, concrete steps are following: the device that HP20 resin bag at first will be housed is put into water body and is adsorbed Microcystin; And then the Microcystin that will be adsorbed on the HP20 resin carries out wash-out with 75% methanol solution; At last the Microcystin of wash-out is analyzed with high performance liquid chromatography or liquid chromatograph mass spectrography system.
The above-mentioned device that the HP20 resin is housed is characterized in that, includes the permeable absorbent packet of ability that the HP20 resin is housed, and described absorbent packet is placed in the protector that has permeable hole, and below protector, is connected with settler.
Above-mentioned protector is spherical.
The present invention handles and efficient liquid phase chromatographic analysis in conjunction with the desorption of toxin through the in-situ acquisition Microcystin, realizes real-time monitoring and early warning to potable water seedbed Microcystin.Method of the present invention is simple to operate, cost is lower, has avoided the bio-transformation of toxin composition, and the sample substrate after the processing is pure, helps the qualitative and quantitative analysis of chromatographic technique.Simultaneously, this method is compared with the biological monitoring method with traditional water sample analysis, and the Microcystin that can monitor in advance in the water body pollutes, and sensitivity is higher, can realize the early warning to potable water seedbed water quality safety.The apparatus structure that uses in the inventive method is ingenious, can effectively make HP20 resin adsorption Microcystin, has the excellent popularization using value.
Description of drawings
Fig. 1: the perspective view of apparatus of the present invention;
Fig. 2: the diagrammatic cross-section of apparatus of the present invention
Wherein 1, nylon rope 2, protector 3, permeable hole 4, settler 5, absorbent packet 6, screw.
Embodiment
Facing method of the present invention and used device down is described in detail:
Embodiment:
2g HP20 resin bag at first will be housed put into microcystic aeruginosa nutrient solution absorption Microcystin 1h, 1d, 2d, 4d, 7d; The HP20 resin bag of absorbing toxin is cut off then, with 4mL 75% methanol solution resin is flushed in the 7mL centrifuge tube, behind the concussion 30min, uses hydro-extractor 8000rpm, and the 10min centrifugal treating is got supernatant and crossed 0.22 μ m filter membrane, and is to be measured;
Testing sample is analyzed with high performance liquid chromatography; In the monitoring for Microcystin; The selection of moving phase and proportioning have tangible influence for monitoring result, and the applicant finds in long term studies, when moving phase is: the mixed solution of acetonitrile, water and trifluoroacetic acid; Acetonitrile wherein: water: during trifluoroacetic acid=35: 64.95: 0.05 (volume ratio), the result that the Microcystin of concentration known is detected shows that the detection accuracy rate of above-mentioned moving phase is the highest.
Table 1: the detection effect of the inventive method
Figure BDA0000140979340000021
The result of this instance shows (seeing table 1), utilizes in the monitoring water body that this method can be successful whether contain Microcystin.
Below in conjunction with accompanying drawing invention is further specified.
In the drawings, include nylon rope 1, protector 2 (long diameter 20cm, short diameter 15cm), permeable hole (aperture 0.3cm) 3, settler 4, absorbent packet 5 (3cm * 3cm) and screw 6.Absorbent packet 5 ties up on the nylon rope 1, and the protector 2 of the sphere that one of outer mask can be permeable is made up of two hemisphere; And be fixed together with screw 6; In order to protect the absorbent packet 5 in it, settler 4 hangs over the lower end of protector 2, and rope 1 upper end is fixed on buoy or other is above platform.When using, put into protector 2 after packing into the HP20 resin in the absorbent packet 5, sink to absorbing toxin in the water body to be monitored.

Claims (6)

1. the in-situ monitoring method of a Microcystin is characterized in that it being to come the Microcystin in the adsorbed water body with the HP20 resin.
2. monitoring method as claimed in claim 1, concrete steps are following: the device that HP20 resin bag at first will be housed is put into water body and is adsorbed Microcystin; And then the Microcystin that will be adsorbed on the HP20 resin carries out wash-out with 75% methanol solution; Microcystin with wash-out carries out concentration analysis with high performance liquid chromatography or liquid chromatograph mass spectrography system at last.
3. monitoring method as claimed in claim 1, the moving phase that it is characterized in that described high performance liquid chromatography or liquid chromatograph mass spectrography system is the mixed solution of acetonitrile, water and trifluoroacetic acid.
4. monitoring method as claimed in claim 1 is characterized in that acetonitrile in the mixed solution of described acetonitrile, water and trifluoroacetic acid: water: trifluoroacetic acid=35: 64.95: 0.05.
5. be used to be equipped with the device of HP20 resin, it is characterized in that, include the permeable absorbent packet of ability that the HP20 resin is housed, described absorbent packet is placed in the protector that has permeable hole, and below protector, is connected with settler.
6. device as claimed in claim 5 is characterized in that described protector is for spherical.
CN201210056845.3A 2012-03-06 2012-03-06 Method and device for in-situ monitoring of microcystin Expired - Fee Related CN102608239B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201210056845.3A CN102608239B (en) 2012-03-06 2012-03-06 Method and device for in-situ monitoring of microcystin

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Application Number Priority Date Filing Date Title
CN201210056845.3A CN102608239B (en) 2012-03-06 2012-03-06 Method and device for in-situ monitoring of microcystin

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CN102608239A true CN102608239A (en) 2012-07-25
CN102608239B CN102608239B (en) 2014-10-29

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103217388A (en) * 2013-04-01 2013-07-24 浙江大学 Method for carrying out water quality monitoring by utilizing waste ion exchange resin ball
CN107941925A (en) * 2017-11-15 2018-04-20 新疆大学 A kind of liquid phase adsorption assay method in real time in situ

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
王中婵等: "大孔吸附树脂分离纯化微囊藻毒素", 《环境科学学报》 *
***: "水体浮游植物浓度原位分类测量方法研究与***研制", 《中国科技大学博士学位论文》 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103217388A (en) * 2013-04-01 2013-07-24 浙江大学 Method for carrying out water quality monitoring by utilizing waste ion exchange resin ball
CN103217388B (en) * 2013-04-01 2015-04-29 浙江大学 Method for carrying out water quality monitoring by utilizing waste ion exchange resin ball
CN107941925A (en) * 2017-11-15 2018-04-20 新疆大学 A kind of liquid phase adsorption assay method in real time in situ
CN107941925B (en) * 2017-11-15 2020-07-14 新疆大学 In-situ real-time liquid phase adsorption determination method

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