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Method used for rapid separation and detection of organophosphorus pesticides in water

A technology for organophosphorus pesticides and water determination, which is applied in material separation, measurement devices, analytical materials, etc., can solve the problems of difficult extraction of biological enzymes, complicated operations, easy inactivation of enzyme activities, etc., and achieves low-cost laboratory and on-site detection. The effect of universal practicability and improved specific surface area

Active Publication Date: 2015-07-15
MINNAN NORMAL UNIV
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Problems solved by technology

The detection of organophosphorus pesticides in the national standard method is mainly GC. Although the sensitivity and selectivity of quantitative analysis of these methods are high, the measurement results are reliable and the reproducibility is good, there are some shortcomings, such as their complicated operation, expensive reagents, and sample Pretreatment is required, and skilled technicians and expensive equipment are required. It is impossible to realize on-site detection and it is impossible to realize popular use at home, so the actual use value is not high.
Some researchers also introduced acetylcholinease into thin-layer chromatography to achieve rapid detection, but there are still some defects, such as: the simultaneous detection of multiple organophosphorus pesticides cannot be realized, and the extraction of acetylcholinease is complicated, the extraction amount is small, and the extraction cost is high. It is difficult to achieve mass production , the enzyme activity is easily inactivated
Such as the extraction of biological enzymes in the organophosphorus pesticide rapid detection test paper disclosed in Chinese Patent Application No. 200710052773.4 is difficult, easily loses activity, and is limited in actual use; Require

Method used

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  • Method used for rapid separation and detection of organophosphorus pesticides in water
  • Method used for rapid separation and detection of organophosphorus pesticides in water
  • Method used for rapid separation and detection of organophosphorus pesticides in water

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preparation example Construction

[0038] Step 2, preparation of photocatalytic thin-layer chromatography plate:

[0039] Weigh a certain amount of TiO modified with ascorbic acid 2 (Particle size is 500nm), silica gel G, 0.5% (m / v) sodium carboxymethyl cellulose, stir evenly (the mass ratio of the three is 2:3:14), spread on a 2.5×10cm glass plate, put In an electric thermostat blast drying oven, dry at 50-60°C and activate at 105-110°C for half an hour to make a thin-layer chromatographic plate such as Figure 5 shown;

[0040] Step 3, chromatographic separation and chromogenic determination of organophosphorus pesticides:

[0041]Draw a sample starting line on the activated TLC plate at 10mm from the starting end, and the sample volume is 20-50uL; use a pipette to pipette n-hexane:acetone:methanol:water=5:2:1.5: Put 10mL of 1.5 (v / v) mixed developing agent in the developing cylinder, put the printed TLC plate into the developing cylinder, cover the cylinder cover to avoid light and perform chromatography ...

Embodiment

[0044] In order to verify the applicability of the method of the present invention, the applicant carried out separation and determination according to the organophosphorus pesticide specified in the domestic application water standard (GB5749-2006): weigh ascorbic acid modified TiO 2 (Particle size is 500nm), silica gel G, 0.5% sodium carboxymethyl cellulose (the mass ratio of the three is 2:3:14) and stir evenly, spread it on a 2.5×10cm glass plate, put it into the electric heating constant temperature blast drying In the box, dry at 60°C and activate at 105°C for half an hour to make a thin-layer chromatography plate; draw a starting line for spotting the sample at the starting end of the thin-layer chromatography plate at 10mm, and pipette the normal Alkane: acetone: methanol: water = 5:2:1.5:1.5 (v / v) mixed developer 10mL, placed in a developing cylinder, take 50μL concentration as a certain concentration (0.02mg / L, 0.05mg / L, 0.1 mg / L, 0.2mg / L, 0.6mg / L) of mixed pesticide...

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Abstract

The invention discloses a method used for rapid separation and detection of organophosphorus pesticide in water. The method comprises following steps: an appropriate amount of surface modified TiO2 with a particle size of 500nm, silica gel G and sodium carboxymethylcellulose are mixed and stirred uniformly; a glass plate of 2.5*10cm is coated with the mixture, is dried and activated for half an hour at a temperature of 105 DEG C so as to obtain a thin-layer chromatography plate; a mixture of hexane, acetone, methanol and water is taken as a developing solvent, and it is possible to separate six kinds of organophosphorus pesticides including chlopyrifos, malathion, parathion, methyl parathion, phoxim, and methamidophos by 12min of chromatography in dark; and the organophosphorus compounds are degraded to phosphates after 15 to 20min of sun light treatment, and the phosphates are subjected to color development in dark. Standard solution of each organophosphorus pesticide is prepared in a corresponding linear concentration range, thin-layer chromatography sample plates prepared under the same conditions are used as reference chromatograms, and kind and concentration of the organophosphorus pesticides in water samples can be determined by comparison. The linear concentration range is 0.02mg / L to 0.6mg / L, and detection requirements of drinking water are satisfied.

Description

technical field [0001] The invention relates to an environmental water sample processing technology, in particular to a method for rapidly separating and measuring various organophosphorus pesticides in the environmental water sample. Background technique [0002] Organophosphorus pesticides (Ops) are widely used in agricultural production such as preventing pests and increasing crop yields all over the world, but there are still some hazards: OPs are generally toxic substances that will pollute the environment, especially in order to improve insecticidal effects. Phosphorus pesticides, because the pesticides are stable and difficult to be decomposed, lead to a large amount of organophosphorus pesticides remaining in environmental water bodies or crops. After the human body ingests them, it will inhibit the activity of acetylcholinesterase, resulting in a large accumulation of acetylcholine in human tissues. Choline can be affected The disorder of body activity will cause th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/90
Inventor 李顺兴郑凤英梁文杰
Owner MINNAN NORMAL UNIV
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