CN102426167A

CN102426167A - Photoelectric conversion based rapid detection method for pesticide residual toxicity

Info

Publication number: CN102426167A
Application number: CN201110267497XA
Authority: CN
Inventors: 朱培逸; 徐本连; 高珏; 李鑫; 毛丽民
Original assignee: Changshu Institute of Technology
Current assignee: Changshu Institute of Technology
Priority date: 2011-09-10
Filing date: 2011-09-10
Publication date: 2012-04-25

Abstract

Belonging to the technical field of detection modes for pesticide residual toxicity in food, the invention relates to a photoelectric conversion based rapid detection method for pesticide residual toxicity. The method is characterized by: chopping 2g of a sample for pretreatment, adding 10mL of ultrapure water, introducing a sample valve, adding 2ml of an ionic liquid nbutyl-3-methylimidazole tetrafluoroborate for enrichment and extraction of the sample, subjecting the obtained extracting liquid to separation by a separation column, subjecting the separation liquid with 3ml of an oxidizing agent luminol-hydrogen peroxide system to a chemiluminescence reaction, performing photoelectric conversion through a photomultiplier circuit, amplifying an input electric signal by an amplifying circuit and inputting the signal into a one-chip microcomputer circuit, conducting data analysis and identification on the basis of a database stored in the one-chip microcomputer, then displaying the analysis result on a color screen in the LCD (liquid crystal display) interface circuit by passing it through an LCD control circuit and. Employment of the above technical scheme can make analytical detection of pesticide residual toxicity in vegetables, fruits and other agricultural products very convenient, fast and accurate, and the operation is simple.

Description

Residual toxicity method for quick based on the opto-electronic conversion method

Technical field

The present invention relates to a kind of residual toxicity method for quick, belong to food residual toxicity detection mode technical field based on the opto-electronic conversion method

Background technology

Along with people's is to the continuous concern of food-safety problem, seems most important with the residual toxicity detection problem of the closely bound up vegetable melon and fruit of people's daily life.Show that according to the statistics made by the departments concerned China's agricultural chemicals year use amount broke through 800,000 tons in 2010, occupied first place in the world.The control residues of pesticides are to the harm of human body, and one of effective method is the dynamics of strengthening Detecting Pesticide in the food.Conventional detection majority is that sample is delivered to the laboratory, utilizes specialized equipment to chemically examine detection by the reviewer, and the efficient that wastes time and energy is low.How realizing then and there the vegetable melon and fruit fast detecting, is an existing supervision of being convenient to quality testing department, helps guaranteeing the important topic of common people's food security again.

At present, on the market following several prods is being arranged aspect the residual toxicity of pesticide device:

1. the principle of the GDYN series pesticide residual hazard fast detecting appearance of cygnet Instr Ltd. of Changchun Jilin University are based on agricultural chemicals in the sample to the inhibiting effect of cholinesterase activity and influence the speed of chromogenic reaction, through the mensuration of chromogenic reaction speed being measured wherein residual toxicity amount (being inhibiting rate).Instrument is made up of super brightness silicon radiant, colorimetric pool, integrated electro sensor, temperature sensor, microprocessor and printer, can directly on liquid crystal display, demonstrate the residual toxic dose of agricultural chemicals in the sample, and can directly print testing result.

are the KSJ-4A series portable residual toxicity of pesticide of the fluffy biological medicine company in capital, Shandong incorporated company 2.; Activity with temperature to enzyme changes and the characteristic of variation; Automatically start the alternating temperature program; Make detection not receive the restriction of environment temperature, list is examined about 10 minutes of the time of a sample.

are the HQNC-800 residual toxicity fast measuring appearance of the auspicious emerging Instr Ltd. of Dongguan City 3.; Adopt enzyme to suppress method; According to standard GB/T5009.199-2003 " fast detecting of organophosphorus and carbamate pesticide residue amount in the vegetables " and industry standard NY/448-2001 " organophosphorus and carbamate chemicals for agriculture residual hazard method for quick on the vegetables " development; Six passage detection techniques, the residues of pesticides situation of ability fast detecting agricultural product.

residual toxicity method for quick is to be arranged in the first-line detection technique of basic unit.The detection technique that meets this screening; Must be simple; Existing the said goods is only paid attention to the rapidity that detects on function; The bioanalysis reaction system that generally adopts is complicated, is subject to the influence of activity, medium and the coexistence component of environment temperature, enzyme, and the reliability of analytic signal itself and reappearance exist than wretched insufficiency; Often adopt chromatogram and mass detector etc. in breadboard detection, bring very big difficulty for the instrument microminiaturization

Summary of the invention

the purpose of this invention is to provide a kind of accuracy of detection height, the detection speed residual toxicity method for quick based on the opto-electronic conversion method fast, easy and simple to handle.

the objective of the invention is to reach like this, and a kind of residual toxicity method for quick based on the opto-electronic conversion method is characterized in that: the 2g pretreatment sample is shredded; Add the 10mL ultrapure water; Introduce sampling valve, sample is carried out enrichment and extraction, obtain extract and separate through separating column through the ionic liquid normal-butyl-3-methylimidazole tetrafluoro boric acid that adds 2ml; Parting liquid and 3ml oxygenant luminol-hydrogen peroxide system generation chemiluminescence reaction; Realize opto-electronic conversion through the photomultiplier circuit, input electrical signal is amplified, get into single chip circuit by amplifying circuit; With the database that stores in the single-chip microcomputer to data analyze, identification, with analysis result through showing on the color screen in the LCD interface circuit behind the LCD control circuit.

owing to adopted above technical scheme, makes to destroy poison to carry out analyzing and testing very convenient quick and accurate, easy and simple to handle remaining in agricultural chemicals on the agricultural product such as vegetables, fruit.

Description of drawings

Fig. 1 process flow diagram of the present invention.

The theory diagram of Fig. 2 circuit part of the present invention.

Fig. 3 single chip circuit figure of the present invention.

Fig. 4 power circuit diagram of the present invention.

Fig. 5 clock chip circuit diagram of the present invention.

Fig. 6 serial port circuit figure of the present invention.

Fig. 7 LCD control circuit of the present invention figure.

Fig. 8 LCD interface circuit of the present invention figure.

Fig. 9 photomultiplier circuit diagram of the present invention.

Figure 10 amplification circuit diagram of the present invention.

Figure 11 SD card of the present invention circuit diagram.

Embodiment

are referring to Fig. 1; Because most of agricultural chemicals is independent or composite the processing of agricultural chemicals such as organochlorine class of having been forbidden at present by organophosphorus pesticide, carbamates and part, comprising: the thimet of organic phosphates, demeton, parathion, metrifonate, Rogor, DDVP; The dieldrite of organochlorine class, endrin, D.D.T. (dichloro-diphenyl-trichloroethane), Niran etc.To contain the vegetables of above all kinds of Pesticidal products, the sample chopping of fruit; Adding the 10ml ultrapure water mixes with the ionic liquid at room temperature normal-butyl-3-methylimidazole tetrafluoro boric acid that adds 2ml through sampling valve; Sample is carried out enrichment and extraction; Obtain extract and separate through separating column, parting liquid and 3ml oxygenant luminol-hydrogen peroxide system causes chemiluminescence reaction and produces strong luminescence phenomenon, and the light signal of generation is realized opto-electronic conversion through the photomultiplier circuit; By amplifying circuit input electrical signal is amplified; Get into the single-chip microcomputer of single chip circuit, maintenance data merges and the intelligent optimization technology, realizes analysis, identification to data with the C Programming with Pascal Language; With the correlation parameter database of tens of kinds of common agricultural chemicals that have in the single-chip microcomputer through the mode of comparison analyze intelligently, residual toxicity kind and solubility in the identification fruits and vegetables sample to be measured, again with analysis result through showing on the color screen in the LCD interface circuit behind the LCD control circuit.

are referring to Fig. 2; Circuit part of the present invention comprises: single chip circuit, power circuit, clock chip circuit, serial port circuit, LCD control circuit, LCD interface circuit, amplifying circuit, photomultiplier circuit and SD card circuit; Power circuit provides each circuit power; Single chip circuit is connected with clock chip circuit, serial port circuit, LCD control circuit, amplifying circuit and SD card circuit; The LCD interface circuit is connected with the LCD control circuit, and the photomultiplier circuit is connected with amplifying circuit.

residual toxicity solution causes chemiluminescence reaction with oxygenant and produces strong luminescence phenomenon after extracting, separating; The light signal that produces is realized opto-electronic conversion through the photomultiplier circuit; Through amplifying circuit input single chip circuit; The correlation parameter database that has tens of kinds of common agricultural chemicals in the single chip circuit; Mode through comparison is intelligently analyzed residual toxicity kind and concentration in the fruits and vegetables sample to be measured, analysis result is shown on chip A1 through LCD control circuit input LCD interface circuit again.For the power down protection power supply programmable charge function is provided through clock chip circuit, serial port circuit, and can the charge closing function.The SD card is with after single-chip microcomputer is connected, can with sample information and pesticide sample comparison database all be stored in can the SD card of hot plug in, realize the renewal upgrading of residual toxicity sample comparison database.

are referring to Fig. 3; Single chip circuit comprises Chip Microcomputer A 2, crystal oscillator Y2, resistance R 22 and capacitor C 17-C19; One end of resistance R 22 and capacitor C 19 is connected with 31 pin of Chip Microcomputer A 2; Another termination power VCC of capacitor C 19,3 pin of the termination Chip Microcomputer A 2 of capacitor C 17, crystal oscillator Y2, an end of capacitor C 18 and the other end of crystal oscillator Y2 connect 4 pin of single-chip microcomputer A2; 28 pin of Chip Microcomputer A 2 meet voltage VCC, 12 pin common grounds of the other end of resistance R 22, capacitor C 17, C18 and Chip Microcomputer A 2.A2 is the STC12C5410AD single-chip microcomputer of macrocrystalline scientific & technical corporation.

are referring to Fig. 4; Power circuit is made up of capacitor C 2, electrochemical capacitor C1, C3, C15, C16, diode D1, single lock switch S 5, jack P1 and chip U1, U7; Jack P1 is connected with battery; 1 pin of one termination jack P1 of single lock switch S 5; The anode of another terminating diode D1 of single lock switch S 5, the negative electrode of diode D1 connects the positive pole of electrochemical capacitor C3 and 1 pin of chip U1, and 2 pin of chip U1 are connected back output voltage V CC with the positive pole of an end of capacitor C 2, electrochemical capacitor C1, C16 and 1 pin of chip U7; 2 pin of chip U7 are connected back output voltage V D3.3, the 2 pin common grounds of 3 pin of the negative pole of the other end of capacitor C 2, electrochemical capacitor C1, C3, C15, C16, chip U1, U7 and jack P1 with the positive pole of electrochemical capacitor C15.U1 is a MC7805T voltage stabilizing chip, and U7 is a HT1033 voltage stabilizing chip.

are referring to Fig. 5; The clock chip circuit is made up of resistance R 1, R20, R21, capacitor C 4, crystal oscillator Y1 and chip U2; The 8 pin connecting resistance R1 of chip U2, an end of capacitor C 4; The positive pole of another termination battery BT1 of resistance R 1,7 pin of chip U2 are connected with 6 pin of an end of resistance R 20 and Chip Microcomputer A 2, and 6 pin of chip U2 are connected with 19 pin of an end of resistance R 21 and Chip Microcomputer A 2; 1 pin of the other end of resistance R 20, R21 and chip U2 meets voltage VCC; 5 pin of chip U2 connect 22 pin of single-chip microcomputer A2, and the two ends of crystal oscillator Y1 are connected with 2,3 pin of chip U2 respectively, the 4 pin common grounds of the negative pole of the other end of capacitor C 4, battery BT1 and chip U2.U2 is the DS1302 clock chip.

are referring to Fig. 6; Serial port circuit is made up of capacitor C 5, C7-C10, chip U3 and jack J1, and the end of capacitor C 5, C7 and 16 pin of chip U3 meet voltage VCC, 2 pin of another chip termination U3 of capacitor C 5; The two ends of capacitor C 8 connect 1,3 pin of chip U3 respectively; The two ends of capacitor C 9 connect 4,5 pin of chip U3 respectively, 6 pin of a chip termination U3 of capacitor C 10, and 13,14 pin of chip U3 are 3,2 pin of jointing holes J1 respectively; 11,12 pin of chip U3 are connected with 1,32 pin of Chip Microcomputer A 2 respectively, the 15 pin common grounds of the other end of capacitor C 7, C10, chip U3.U3 is the MAX232 communication chip, communicates through jack J1 and host computer.

are referring to Fig. 7; The LCD control circuit is made up of chip A3; 11,12,14,15,16 pin of chip A3 are connected with 5,21,20,18,17 pin of Chip Microcomputer A 2 respectively; 1,10 pin of chip A3 meet voltage VD3.3, and 2,3,4,5 pin of chip A3 connect the LCD interface circuit, the 6 pin ground connection of chip A3.A3 is an ADS7843 touch-screen chip.

are referring to Fig. 8; The LCD interface circuit is made up of resistance R 9-R14, triode Q1, chip A1 and connector JP1; 2,3 pin of one end of resistance R 9,1 pin of connector JP1 and chip A1 meet VD3.3; 35,36 pin of chip A1 meet voltage VCC, and 5,6,7,8 pin of chip A1 connect 20,21,22,24 pin of connector JP1 respectively, and 4 pin of chip A1 connect 19,30 pin of connector JP1; The 9-24 pin of chip A1 connects the 3-18 pin of connector JP1 respectively; The 26-29 pin of chip A1 connects the 5-2 pin of chip A3 respectively, and the end of resistance R 10, R11, R12, R13, R14 connects 30,31,32,33,34 pin of chip A1 respectively, the collector of another termination triode Q1 of resistance R 10, R11, R12, R13, R14; 23 pin of another termination connector JP1 of the base stage of triode Q1 and resistance R 9,1,25, the 37 pin common grounds of 2 pin of the emitter of triode Q1, connector JP1 and chip A1.A1 is an ILI9325 touch-screen chip for driving.

are referring to Fig. 9; The photomultiplier circuit is made up of chip U5, resistance R 7, slide rheostat R8,2 pin of a chip termination U5 of resistance R 7, the end of another termination slide rheostat R8 of resistance R 7; 3 pin of the slip chip termination U5 of slide rheostat R8; 4 pin of chip U5 meet voltage VCC, and 7 pin of chip U5 connect amplifying circuit, 5, the 6 pin common grounds of the other end of slide rheostat R8 and chip U5.U5 is the H9858 chip, and the hole of receiving optical signals is arranged on the shell of core U5, realizes opto-electronic conversion.

are referring to Figure 10; Amplifying circuit is made up of resistance R 4-R6, slide rheostat R3, capacitor C 14, C13 and chip U6; 7 pin of one termination photomultiplier circuit chips U5 of resistance R 4, the other end connecting resistance R5 of resistance R 4, an end of capacitor C 14, another termination slide rheostat R3 of resistance R 5, an end of capacitor C 13 and 2 pin of chip U6; 6 pin of one chip termination U6 of the other end of the sliding end of slide rheostat R3, capacitor C 13, resistance R 6; The other end of resistance R 6 connects 16 pin of single-chip microcomputer A2, and 7 pin of chip U6 meet voltage VCC, 3, the 4 pin common grounds of the other end of capacitor C 14 and chip U6.U6 is the OPA350 chip.

Referring to Figure 11; SD card circuit is made up of SD card and resistance R 25-R29, the termination voltage VCC of 5 pin of SD card and resistance R 25-R29, the other end of 1 pin connecting resistance R25 of SD card; 2 pin of SD card and the other end of resistance R 26 connect 9 pin of single-chip microcomputer A2; 3 pin of SD card and the other end of resistance R 27 connect 23 pin of single-chip microcomputer A2, and 6 pin of SD card connect 25 pin of single-chip microcomputer A2, and 8 pin of SD card and the other end of resistance R 28 connect 24 pin of single-chip microcomputer A2; The other end of 9 pin connecting resistance R29 of SD card, 4,7 pin ground connection of SD card

Claims

1. A kind of residual toxicity method for quick based on the opto-electronic conversion method; It is characterized in that: with the chopping of 2g pretreatment sample, add the 10mL ultrapure water, introduce sampling valve; Ionic liquid normal-butyl-3-methylimidazole tetrafluoro boric acid through adding 2ml carries out enrichment and extraction to sample; Obtain extract and separate through separating column, parting liquid and 3ml oxygenant luminol-hydrogen peroxide system generation chemiluminescence reaction realizes opto-electronic conversion through the photomultiplier circuit; By amplifying circuit input electrical signal is amplified; Get into single chip circuit, with the database that stores in the single-chip microcomputer to data analyze, identification, with analysis result through showing on the color screen in the LCD interface circuit behind the LCD control circuit