CN1271400C - Rapid determination method for organophosphorus pesticide residue in vegetable and fruit - Google Patents
Rapid determination method for organophosphorus pesticide residue in vegetable and fruit Download PDFInfo
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- CN1271400C CN1271400C CN 200310119273 CN200310119273A CN1271400C CN 1271400 C CN1271400 C CN 1271400C CN 200310119273 CN200310119273 CN 200310119273 CN 200310119273 A CN200310119273 A CN 200310119273A CN 1271400 C CN1271400 C CN 1271400C
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Abstract
The present invention relates to a method for measuring the organophosphorus pesticide residue in fruits and vegetables. Organophosphorus pesticide in fruits and vegetables is extracted with an organic solvent, and a phosphorous coextraction material of non-organophosphorus pesticide in extraction liquid is removed by utilizing an adsorbing agent to eliminate interference; a solvent in the purified extraction liquid is just blown off completely with air or nitrogen, potassium persulfate solution is added into residue and processed through sealing digestion to convert the organophosphorus pesticide into orthophosphate; finally, molybdenum antimony spectrophotometry is used to determine the concentration of the orthophosphate in digested solution; thereby, the total residue of the organophosphorus pesticide in fruit and vegetable samples is calculated. The present invention has the advantages of rapid measuring speed, high precision, stability and reliability, simple and cheap device and low measuring cost. A measuring result has good consistency with a measuring result by gas chromatography; a detection limit is low; the detection limit to various kinds of organophosphorus pesticide is 0.05 to 0.1 mg/kg.
Description
(1) technical field
The present invention relates to the assay method of organophosphorus pesticide residual quantity in a kind of fruits and vegetables.
(2) background technology
At present, the assay method of organophosphorus pesticide mainly contains vapor-phase chromatography and enzyme inhibition method in the fruits and vegetables.Vapor-phase chromatography result is accurate, but needs expensive instrument, skilled operating personnel, and operates loaded down with trivial detailsly, time-consuming, consumes a large amount of organic solvents.Comprise sample pretreatment, analyzing single sample needed about 2 hours and nearly hundred milliliters of solvents.Vapor-phase chromatography generally is used as standard method or referee method, and should not be used for the fast measuring of a large amount of sample organophosphorus pesticides.The advantage that enzyme suppresses method is that cost is low, consuming time few, and the mensuration expense of single sample needs several units, time-consuming 15～30 minutes approximately.Enzyme inhibition method can be applicable to the fast measuring of organophosphorus and carbamate pesticide residue in the vegetables.But the sensitivity of this method is generally not high, and the source of measurement result and employed enzyme, chromogenic reaction and reaction time, temperature of reaction have confidential relation, is disturbed easily and omission and flase drop phenomenon occur.The detectability of this method has very big difference because of the difference of pesticide variety, and the measurement result correlativity of measurement result and vapor-phase chromatography is poor, often the real persticide residue in the response sample.
(3) summary of the invention
The objective of the invention is to be mainly the market of farm produce and fruit and vegetable production base provides a kind of highly sensitive, can fast and accurately measure the method for organophosphorus pesticide residual quantity in the fruits and vegetables.
The said assay method of the present invention is as follows:
1) extraction
With vegetables or fruit chopping or rubbing, take by weighing 5～15g in centrifuge tube, add the organic solvent of 5～15g anhydrous sodium sulfate and 10～20ml, extraction 2～3min transfers to extract in another centrifuge tube; Said organic solvent is at least a in acetone, ethyl acetate and the methylene chloride;
2) purify
Add the anhydrous sodium sulfate of 2～5g and the activated charcoal of 0.01～0.2g in the centrifuge tube that extract is housed, vibration 1～2min leaves standstill the back and draws upper solution, filters to remove to be suspended in activated charcoal in the solution, and filtrate being collected in cleared up in the test tube;
3) concentrate
To place temperature be 35～70 ℃ water-bath with the test tube of clearing up that filtrate is housed, and the solvent in the test tube purged clean with nitrogen or air;
4) clear up
Adding concentration is potassium persulfate solution 1～2ml of 2%～5% (W/V) in the test tube toward clearing up, the test tube sealing is placed on to heat on the counteract appearance clears up, and 150～170 ℃ of digestion conditions, digestion time 8～15min, organophosphorus pesticide all are converted into orthophosphate:
5) measure
Measure the concentration (C of phosphorus in the solution after clearing up with molybdenum-antimony anti-spectrophotometric method
p, μ g/ml), can calculate the total residue of organophosphorus pesticide in the sample by following formula:
Wherein C is the total residue (mg/kg) of organophosphorus pesticide in the laboratory sample, C
pBe the concentration (μ g/ml) of phosphorus in the solution after clearing up, V is the volume (ml) of potassium persulfate solution used when clearing up, and W is the weight (g) of laboratory sample, the atomic weight of phosphorus is 31, the molecular weight of most of organophosphorus pesticide is between 200-300, and getting its mean molecular weight is 250
The present invention has the following advantages: 1) finding speed is fast, the disposable measures a required time of sample and is about 25min, its extraction, concentrate, clear up, determination step can carry out simultaneously to a plurality of samples, the disposable measures 12 required times of sample and is about 1 hour; 2) accuracy height, its stability and reliability height, the measurement result of measurement result and vapor-phase chromatography has good consistance; 3) detectability is low, and the detection of various organophosphorus pesticides is limited to 0.05～0.1mg/kg.Utilize adsorbent that extract is purified, removed the phosphorous thing that comes together altogether of non-organophosphorus pesticide wherein, make the blank absorbency behind the Specimen eliminating reduce to 0.02～0.04 (2cm light path), thereby obtain very low detectability; 4) equipment is simple, cheap; 5) cost of determination is low, and agents useful for same is common reagent, and low price and easily buying in market is measured the required expense of sample less than 1 yuan.
(4) embodiment
The present invention is further illustrated below by embodiment.
Embodiment 1:
Green vegetables 10g, chopping is in the centrifuge tube of packing into; In centrifuge tube, add 10ml ethyl acetate and 3g anhydrous sodium sulfate, place ultrasonic oscillator to extract 2min centrifuge tube, with micropipettor all extracts are transferred in another centrifuge tube then.In the centrifuge tube that extract is housed, add 2g anhydrous sodium sulfate and 0.025g activated charcoal, vibration 1min leaves standstill behind the 1min and draws the 5ml upper solution with micropipettor, and micropipette tip is directly inserted the syringe-type filtrator, release solution, filter removal and be suspended in activated charcoal in the solution.Filtrate being collected in cleared up in the test tube.To place temperature be 65 ℃ water-bath with the test tube of clearing up that filtrate is housed, and purges the ethyl acetate in the test tube clean just fully with pressurized air.
Adding concentration is the potassium persulfate solution 1ml of 4% (W/V) in the test tube toward clearing up, the test tube sealing is placed on to heat on the counteract appearance clears up, and 170 ℃ of digestion conditions, digestion time 8min, organophosphorus pesticide all are converted into orthophosphate.The concentration of measuring phosphorus in the solution after clearing up with molybdenum-antimony anti-spectrophotometric method is 0.12 μ g/ml, and the total residue that calculates organophosphorus pesticide in the laboratory sample thus is 0.19mg/kg.Owing to use the ethyl acetate extraction of 10ml in the present embodiment, the extract of 5ml is measured, and therefore the weight w of laboratory sample should be 5g when calculating.
Embodiment 2:
The orange chopping of peeling is got 5g and is packed in the centrifuge tube, and adding 10ml ethyl acetate and 10g anhydrous sodium sulfate in the centrifuge tube place ultrasonic oscillator to extract 2min centrifuge tube, with micropipettor all extracts are transferred in another centrifuge tube then.In the centrifuge tube that extract is housed, add 2g anhydrous sodium sulfate and 0.05g activated charcoal, vibration 1min leaves standstill behind the 1min and draws the 5ml upper solution with micropipettor, and micropipette tip is directly inserted the syringe-type filtrator, release solution, filter removal and be suspended in activated charcoal in the solution.Filtrate being collected in cleared up in the test tube.
To place temperature be 65 ℃ water-bath with the test tube of clearing up that filtrate is housed, and purges the ethyl acetate in the test tube clean just fully with pressurized air.Adding concentration is the potassium persulfate solution 1ml of 4% (W/V) in the test tube toward clearing up, the test tube sealing is placed on to heat on the counteract appearance clears up, and 170 ℃ of digestion conditions, digestion time 10min, organophosphorus pesticide all are converted into orthophosphate.The concentration of measuring phosphorus in the solution after clearing up with molybdenum-antimony anti-spectrophotometric method is 0 μ g/ml, and the total residue that calculates organophosphorus pesticide in the laboratory sample thus is 0mg/kg.
Claims (2)
1. the rapid assay methods of organophosphorus pesticide residual quantity in vegetables and the fruit is characterized in that its step is as follows:
1) extraction with vegetables or fruit chopping or rubbing, takes by weighing 5～15g in centrifuge tube, adds the organic solvent of 5～15g anhydrous sodium sulfate and 10～20ml, and extraction 2～3min transfers to extract in another centrifuge tube; Said organic solvent is at least a in acetone, ethyl acetate and the methylene chloride;
2) purify, add the anhydrous sodium sulfate of 2～5g and the activated charcoal of 0.01～0.2g in the centrifuge tube that extract is housed, vibration 1～2min leaves standstill the back and draws upper solution, filters to remove to be suspended in activated charcoal in the solution, and filtrate being collected in cleared up in the test tube;
3) concentrate, to place temperature be 35～70 ℃ water-bath with the test tube of clearing up that filtrate is housed, and the solvent in the test tube purged clean with nitrogen or air;
4) clear up, to add W/V concentration be potassium persulfate solution 1～2ml of 2%～5% toward clearing up in the test tube, the test tube sealing is placed on the counteract appearance heating clears up 150～170 ℃ of digestion conditions, digestion time 8～15min, organophosphorus pesticide all are converted into orthophosphate;
5) measure, the concentration of phosphorus in the solution after clearing up with molybdenum-antimony anti-spectrophotometric method mensuration, unit is μ g/ml, is calculated the total residue of organophosphorus pesticide in the sample by following formula:
Wherein C is the total residue of organophosphorus pesticide in the laboratory sample, and unit is mg/kg, C
pBe the concentration of phosphorus in the solution after clearing up, unit is μ g/ml, and V is the volume of potassium persulfate solution used when clearing up, and unit is ml, and W is the weight of laboratory sample, and unit is g.
2, the rapid assay methods of organophosphorus pesticide residual quantity in vegetables as claimed in claim 1 and the fruit is characterized in that said time of repose is 1～2min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310119273 CN1271400C (en) | 2003-12-02 | 2003-12-02 | Rapid determination method for organophosphorus pesticide residue in vegetable and fruit |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310119273 CN1271400C (en) | 2003-12-02 | 2003-12-02 | Rapid determination method for organophosphorus pesticide residue in vegetable and fruit |
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| CN1546988A CN1546988A (en) | 2004-11-17 |
| CN1271400C true CN1271400C (en) | 2006-08-23 |
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| CN 200310119273 Expired - Fee Related CN1271400C (en) | 2003-12-02 | 2003-12-02 | Rapid determination method for organophosphorus pesticide residue in vegetable and fruit |
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Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101241113B (en) * | 2007-02-07 | 2010-12-22 | 劲牌有限公司 | Chinese herbal medicine residual organophosphorus pesticide detection method |
| CN101246149B (en) * | 2008-03-25 | 2011-04-20 | 中国检验检疫科学研究院 | Fast high-precision detecting method for animal medicine residue in food |
| CN101363783B (en) * | 2008-09-10 | 2010-12-15 | 东北农业大学 | Clarificant for preprocessing emulsion and method for preparing same |
| US8426212B2 (en) * | 2010-10-06 | 2013-04-23 | The Boeing Company | Method and system for monitoring for the presence of phosphate esters in jet fuel |
| CN103196886A (en) * | 2013-03-20 | 2013-07-10 | 厦门大学 | Detection method of organophosphorus pesticide residues in tea |
| CN105116069A (en) * | 2015-08-24 | 2015-12-02 | 上海睿致生物科技有限公司 | Reagent and method for rapidly testing pesticide residues |
| CN105572098A (en) * | 2016-01-12 | 2016-05-11 | 厦门大学 | Rapid detection method for residual trithion in fruits and vegetables |
| CN107831257A (en) * | 2017-10-27 | 2018-03-23 | 无锡艾科瑞思产品设计与研究有限公司 | A kind of organophosphorus residue quantity measuring method |
| CN108279232A (en) * | 2018-01-23 | 2018-07-13 | 浙江大学 | Rice phosphorus content rapid screening method |
| CN108872139A (en) * | 2018-05-09 | 2018-11-23 | 苏州农业职业技术学院 | Organophosphorus pesticide detection method in a kind of vegetable and fruit |
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