CN1632538A - Fast detection method with high sensitivity for pesticide residue - Google Patents

Abstract

It is a rapid and accurate test method of pesticide remains, which is characterized by the following: to use fluorescence probe as indicator to give the suppression degree to choline kinase activity of the organic phosphor pesticide and amidocarbonic acid pesticide or to give the process of the hydrolase reaction of the organic phosphor; to test the pesticide remains through the changes of the fluorescence intensity. This invention provides a new method of high accurate pesticide remains, which can achieve the limit of 2mug/kg of the pesticide of the organic phosphor and amidocarbonic acid.

Description

A kind of residues of pesticides high sensitivity method for quick

Technical field:

The invention belongs to analyzing and testing new method and new principle, particularly utilize the fluorescence probe means to detect the new principle of trace residues of pesticides.

Background technology:

Organophosphorus pesticide and carbamic acid lipid agricultural chemicals are respectively China's second generation and third generation pesticide, and the organo-chlorine pesticide of the first generation has stopped producing in China.According to statistics, organophosphorus in 1994 and carbamate insecticides account for 57% of world market, and as seen its consumption is big.In recent years, because the abuse of organophosphorus and carbamate chemicals for agriculture or excess use, have the incident that acute poisoning takes place remains of pesticide and happen occasionally because of eating by mistake.At present, various types of pesticide residue rapid detector kinds are more, but all have the lower problem of sensitivity, and the agricultural product that contain remains of pesticide are difficult to effective control.

Summary of the invention:

The purpose of this invention is to provide a kind of highly sensitive Fast Determination of Pesticide Residue method.

The invention provides a kind of residues of pesticides high sensitivity method for quick, it is characterized in that:

As indicator, indication organophosphorus pesticide and carbamic acid lipid agricultural chemicals suppress degree to activity of cholinesterase, perhaps indicate the process of described agricultural chemicals to the organophosphor hydrolytic enzyme hydrolysis reaction with fluorescence probe;

Persticide residue is measured in variation by fluorescence intensity.

In the residues of pesticides high sensitivity method for quick of the present invention, described enzyme is preferably selected acetylcholine esterase (AChE) for use.

The ultimate principle of residues of pesticides high sensitivity method for quick of the present invention is: organophosphorus pesticide and carbamic acid lipid agricultural chemicals are the inhibitor of CHE (ChE), can with the hydroxyl combination on the activity of cholinesterase central hair propylhomoserin, make CHE phosphorylated or carbamylization, stoped the combination of acetylcholine and CHE, thereby inhibitory enzyme activity causes the variation of pH value; By reacting with the coexistence fluorescence probe, the pH value changes can cause that the fluorescence intensity of fluorescence probe changes; According to the fluorescence probe principle that fluorescence intensity changes under different PH, utilize the fluorescence detector fluorescence intensity, and then measure persticide residue.

Characteristics of the present invention are can fast detecting pesticide residue, has higher sensitivity.At organophosphorus pesticide and carbamic acid lipid agricultural chemicals, be standard substance with the furans pellet, detectability can reach 2 μ g/kg.

Description of drawings:

Fig. 1 is the chromatogram of the red agricultural chemicals of furans;

Fig. 2 is the calibration curve of the red agricultural chemicals of furans.

Embodiment:

The present invention can realize by the following technical solutions:

Liquid chromatographic system comprises the Waters515 liquid chromatography pump, manual pin injector, Waters474 fluorescence detector, excitation wavelength 340-430nm emission wavelength 490-590nm, the capillary column of 500mm * 0.5mm, chromatographic work station.

The present invention can realize by Flow Injection Analysis method and fluorophotometric method equally:

The liquid chromatographic system analysis condition:

Flow velocity: 0.8ml/min

Temperature: constant temperature (25 ℃)

Sample size: 10 μ L

Embodiment 1, the calibration curve of the red agricultural chemicals of furans

With the furans pellet is standard substance, use the red standard solution of furans of the 0.05M phosphate buffer solution preparation variable concentrations of pH=7, after respectively getting 20 μ l and 20 μ l enzymes mix according to the batch sampling system ultimate density: 0.47 μ g/kg, 0.94 μ g/kg, 1.88 μ g/kg, 4.7 μ g/kg, 9.42 μ g/kg, 18.84 μ g/kg, 23.56 μ g/kg, 31.2 μ g/kg, 47.1 μ g/kg.Sample introduction obtains peak shape such as accompanying drawing 1 successively.

Obtain calibration curve such as accompanying drawing 2.Calibration curve R ²=0.999, method detectability 2ug/kg (calculating) to suppress 10%.

Claims (2)

1, a kind of residues of pesticides high sensitivity method for quick is characterized in that:

As indicator, indication organophosphorus pesticide and carbamic acid lipid agricultural chemicals suppress degree to activity of cholinesterase, perhaps indicate the process of described agricultural chemicals to the organophosphor hydrolytic enzyme hydrolysis reaction with fluorescence probe;

Persticide residue is measured in variation by fluorescence intensity.

2, according to the described residues of pesticides high sensitivity of claim 1 method for quick, it is characterized in that: described enzyme is an acetylcholine esterase.

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