CN103439437A - Gas chromatography detection method of residual quantity of pesticide dichlorvos in vegetables and fruits - Google Patents
Gas chromatography detection method of residual quantity of pesticide dichlorvos in vegetables and fruits Download PDFInfo
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- CN103439437A CN103439437A CN2013104054222A CN201310405422A CN103439437A CN 103439437 A CN103439437 A CN 103439437A CN 2013104054222 A CN2013104054222 A CN 2013104054222A CN 201310405422 A CN201310405422 A CN 201310405422A CN 103439437 A CN103439437 A CN 103439437A
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Abstract
The invention builds a gas chromatography method for detecting the residual quantity of pesticide dichlorvos in vegetables and fruits. The gas chromatography method for detecting the residual quantity of the pesticide dichlorvos in vegetables and fruits is characterized in that acetonitrile is used as an extracting agent, in the purification and concentration processes of exacted liquid, the bath temperature of a nitrogen blowing instrument is controlled to be 45-50 DEG C, the nitrogen or air flow is blown to the surface of a sample along the wall of a test tube (a stainless steel air needle is tightly attached to the wall of the test tube), when a solvent sample is evaporated and concentrated to 0.5ml to 1ml, acetone is immediately added for fixing the volume, anhydrous sodium sulfate is added for dehydrating, and the supernate is taken and subjected to trace analysis by a gas chromatograph. The method has the advantages of simple and convenient operation, rapid analysis, accurate result, dichlorvos fortified recovery of 95.2%-99.6% and variable coefficient of less than 3.9%.
Description
Technical field
The present invention sets up a kind of gas chromatography that detects DDVP agricultural chemicals residual quantity in vegetables, fruit, belongs to the Detection Technologies of Pesticide Residues field.
Background technology
DDVP is a kind of efficient, wide spectrum, quick-acting organophosphorus insecticide, its chemical name is O, O-dimethyl-O-(2,2-dichloroethylene) phosphate, it has strong stifling, stomach toxicity and action of contace poison, and biting mouthparts and sucking pest are all had to prevention effect preferably.Be widely used in the pest control of cotton, fruit tree, vegetables and tobacco, be use with a long history, one of agricultural chemicals that amount of application is large, wide.
The DDVP volatility is large, 74 ℃ of sterling boiling points (under 133.322Pa), and easily volatilization voluntarily, be the strongest kind of fumigation action in organophosphorus insecticide at normal temperatures.
In application NY/T761-2008 detects vegetables and fruit, during the DDVP residues of pesticides, because the DDVP boiling point is low, polarity is stronger, in the pretreatment process of sample, composition DDVP loss percentage to be measured is very high, causes the testing result accuracy low, recovery of standard addition is everlasting below 50%, even lower.
The present invention sets up a kind of gas chromatography that detects DDVP residual quantity in vegetables, fruit, and accuracy is high, adds the recovery and reaches 95.2%-99.6%.
Summary of the invention
The present invention has following two aspects:
1, sample pre-treatments
2, gas chromatograph detects
The technology used in the present invention comprises following content:
(1) preparation of sample
Get the edible part of fresh vegetables, fruit sample, by its chopping, fully mix and put into the food processing equipment pulverizing, make sample to be checked.
(2) instrument and reagent
1. instrument Agilent6890 gas chromatograph, is furnished with flame photometric detector (FPD) (FPD), DB-608 (30m * 0.32mm * 0.5 μ m) capillary chromatographic column, HP-5 (30m * 0.32mm * 0.25 μ m) capillary chromatographic column, electronic balance, Germany IKA high-speed homogenization machine, U.S. N-EVAP24 water-bath Nitrogen evaporator.
2. reagent acetonitrile, sodium chloride (140 ℃ of baking 4h), anhydrous sodium sulfate (in 650 ℃ of muffle furnaces, drying 6h) reagent are and analyze purely, and acetone reagent is the import chromatographically pure.
3. pesticide standard sample DDVP standard solution is purchased from Inst. of Environment Protection & Scientific Research Monitor, Ministry of Agric, and mass concentration is 100 μ g/ml.
(3) sample pre-treatments
1. extract and accurately take the 25.0g sample in the 250ml beaker, add the 50ml acetonitrile, use Filter paper filtering after refiner high speed homogenate 2min, filtrate collecting is equipped with in the 100ml tool plug graduated cylinder of 7g-10g sodium chloride, collect filtrate, cover stopper, concuss 2min, at room temperature standing 30min, make acetonitrile phase and water layering;
2. purify a. and draw the 10.0ml acetonitrile solution from tool plug graduated cylinder, put into 10ml scale test tube; B. test tube is put into to water-bath and heat, bath temperature is controlled at 45 ℃-50 ℃; C. the stainless steel vent wire of Nitrogen evaporator is close to test tube wall, nitrogen or air stream blow to sample surfaces (if the air-flow that the excess Temperature of water-bath, vent wire blow out is excessive, all can reduce the DDVP recovery) along test tube wall; D. treat the sample solvent volatilization, while being concentrated into 0.5ml-1ml (sample concentration is to 0.5ml, and the recovery sharply descends), use immediately the acetone constant volume, be settled to 5.0ml, then add the 1.0g anhydrous sodium sulfate dehydration, fully shake up, standing 5min, get supernatant, for gas chromatograph, detects.
(4) gas chromatograph detects
1. chromatographic parameter is set chromatographic column: DB-608, HP-5 fused-silica capillary column as separating column; Carrier gas: high pure nitrogen (purity 99.999%); The combustion gas of detecting device and combustion-supporting gas H
2150ml/min, air 110ml/min; The sample introduction pattern: constant current, flow is 1.8ml/min; Injector temperature: 235 ℃; Detector temperature: 270 ℃; The post heating schedule: 90 ℃ of initial temperatures, keep 1min, rise to 270 ℃ with 35 ℃/min, keep 2min; Input mode: do not shunt; Sample size 1 μ l.
2. the quantitative and qualitative analysis method is come qualitative (confirming with twin columns) with the retention time of DDVP standard solution, with sample peak area and standard solution peak area ratio, comes quantitatively.
(5) method validation
1. linear and scope respectively compound concentration be 0.05,0.1,0.2,0.5,1.0,2.0, the DDVP series standard solution of 5.0mg/kg, by sample introduction successively under above-mentioned chromatographic condition, with chromatographic peak area (y) to concentration of standard solution (x, mg/kg) drawing standard curve, its related coefficient is 0.9992.
2. accuracy, precision are carried out the accuracy of balancing method to add the recovery, carry out the precision of method for expressing with the coefficient of variation (CV).Add the DDVP standard solution in blank vegetable and fruit sample, add concentration and be 0.05,0.1,1.0,5.0mg/kg, 6 repetitions are set simultaneously, added recovery test by aforesaid sample-pretreating method and chromatographic condition again, on 4 interpolation levels, the average interpolation recovery of DDVP is 95.2%-99.6%, and the coefficient of variation is below 3.9%.
3. detection limit has embodied the sensitivity of method.Add with DDVP standard solution stepwise dilution, detected by above-mentioned pre-treating method and instrument condition, with 3 times of noise calculation, recording concentration limit is 0.01mg/kg.
The present invention utilizes the similar principle that mixes, take acetonitrile as extraction agent, extract solution in purification, concentration process, the bath temperature of Nitrogen evaporator is controlled at 45 ℃-50 ℃, and nitrogen or air stream blow to sample surfaces (the stainless steel vent wire is close to test tube wall) along test tube wall, until the sample solvent volatilization, while being concentrated into 0.5ml-1ml, use immediately the acetone constant volume, add anhydrous sodium sulfate dehydration, get supernatant, use the gas chromatograph trace analysis.The advantage of the method is: easy and simple to handle, analyze fast, result is accurate, and the interpolation recovery of DDVP reaches 95.2%-99.6%, and the coefficient of variation is below 3.9%.
Embodiment
Mode 1: the detection of DDVP residual quantity in green vegetables
(1) green vegetables sample pre-treatments
1. extract and accurately take the 25.0g sample in the 250ml beaker, add the 50ml acetonitrile, use Filter paper filtering after refiner high speed homogenate 2min, filtrate collecting is equipped with in the 100ml tool plug graduated cylinder of 7g-10g sodium chloride, collect filtrate, cover stopper, concuss 2min, at room temperature standing 30min, make acetonitrile phase and water layering;
2. purify a. and draw the 10.0ml acetonitrile solution from the letter of tool plug amount, put into 10ml scale test tube; B. test tube is put into to water-bath and heat, bath temperature is controlled at 50 ℃; C. the stainless steel vent wire of Nitrogen evaporator is close to test tube wall, nitrogen or air stream blow to sample surfaces along test tube wall; D. volatilize, while being concentrated into 0.6ml, use immediately the acetone constant volume until sample solvent, be settled to 5.0ml, then add the 1.0g anhydrous sodium sulfate dehydration, fully shake up, standing 5min, get supernatant, for gas chromatograph, detects.
(2) gas chromatograph detects
1. chromatographic parameter is set chromatographic column: DB-608, HP-5 fused-silica capillary column as separating column; Carrier gas: high pure nitrogen (purity 99.999%); The combustion gas of detecting device and combustion-supporting gas H
2150ml/min, air 110ml/min; The sample introduction pattern: constant current, flow is 1.8ml/min; Injector temperature: 235 ℃; Detector temperature: 270 ℃; The post heating schedule: 90 ℃ of initial temperatures, keep 1min, rise to 270 ℃ with 35 ℃/min, keep 2min; Input mode: do not shunt; Sample size 1 μ l.
2. the quantitative and qualitative analysis method is come qualitative (confirming with twin columns) with the retention time of DDVP standard solution, with sample peak area and standard solution peak area ratio, comes quantitatively.
(3) accuracy of method and precision
Get blank green vegetables sample and carry out the experiment of the DDVP interpolation recovery, interpolation concentration is 0.05mg/kg, 0.1mg/kg, 1.0mg/kg, a 5.0mg/kg4 level, and each is processed and repeats 6 times.Result: the average recovery rate of DDVP is 95.3%-99.5% (in Table 1), and the coefficient of variation is 2.8%-3.9%, has reached the testing requirement of remains of pesticide fully.
The interpolation recovery of DDVP variable concentrations in table 1 green vegetables
Mode 2: the detection of DDVP residual quantity in honey peach
(1) sample pre-treatments
Identical with mode 1.
(2) chromatogram detects
Identical with mode 1.
(3) accuracy of method and precision
Get blank honey peach sample and carry out the experiment of the DDVP interpolation recovery, interpolation concentration is 0.05mg/kg, 0.1mg/kg, 1.0mg/kg, a 5.0mg/kg4 level, and each is processed and repeats 6 times.Result: the average recovery rate of DDVP is 95.2%-99.6% (in Table 2), and the coefficient of variation, at 1.8%-3.8%, has reached the testing requirement of remains of pesticide fully.
The interpolation recovery of DDVP variable concentrations in table 2 honey peach
Claims (6)
1. a gas chromatography that detects DDVP agricultural chemicals residual quantity in vegetables, fruit, is characterized in that comprising the steps:
1. extract and accurately take the 25.0g sample in the 250ml beaker, add the 50ml acetonitrile, use Filter paper filtering after refiner high speed homogenate 2min, filtrate collecting is equipped with in the 100ml tool plug graduated cylinder of 7g-10g sodium chloride, collect filtrate, cover stopper, concuss 2min, at room temperature standing 30min, make acetonitrile phase and water layering;
2. purify a. and draw the 10.0ml acetonitrile solution from tool plug graduated cylinder, put into 10ml scale test tube; B. test tube is put into to water-bath and heat, bath temperature is controlled at 45 ℃-50 ℃; C. the stainless steel vent wire of Nitrogen evaporator is close to test tube wall, nitrogen or air stream blow to sample surfaces along test tube wall; D. volatilize, while being concentrated into 0.5ml-1ml, use immediately the acetone constant volume until sample solvent, be settled to 5.0ml, then add the 1.0g anhydrous sodium sulfate dehydration, fully shake up, standing 5min, get supernatant, for gas chromatograph, detects;
3. chromatographic parameter is set chromatographic column: DB-608, HP-5 fused-silica capillary column as separating column; Carrier gas: high pure nitrogen (purity 99.999%); The combustion gas of detecting device and combustion-supporting gas H
2150ml/min, air 110ml/min; The sample introduction pattern: constant current, flow is 1.8ml/min; Injector temperature: 235 ℃; Detector temperature: 270 ℃; The post heating schedule: 90 ℃ of initial temperatures, keep 1min, rise to 270 ℃ with 35 ℃/min, keep 2min; Input mode: do not shunt; Sample size 1 μ l;
4. the quantitative and qualitative analysis method is come qualitative (confirming with twin columns) with the retention time of DDVP standard solution, with sample peak area and standard solution peak area ratio, comes quantitatively.
2. a kind of gas chromatography that detects DDVP agricultural chemicals residual quantity in vegetables, fruit according to claim 1, is characterized in that with acetonitrile as extraction agent.
3. a kind of gas chromatography that detects DDVP agricultural chemicals residual quantity in vegetables, fruit according to claim 1, is characterized in that in sample purification, concentration process, and the bath temperature of Nitrogen evaporator is controlled at 45 ℃-50 ℃.
4. a kind of gas chromatography that detects DDVP agricultural chemicals residual quantity in vegetables, fruit according to claim 1, it is characterized in that in sample purification, concentration process, the stainless steel vent wire of Nitrogen evaporator is close to test tube wall, and nitrogen or air stream blow to sample surfaces along test tube wall.
5. a kind of gas chromatography that detects DDVP agricultural chemicals residual quantity in vegetables, fruit according to claim 1, while it is characterized in that sample concentration to 0.5ml-1ml, use the acetone constant volume immediately, adds anhydrous sodium sulfate dehydration.
6. a kind of gas chromatography that detects DDVP agricultural chemicals residual quantity in vegetables, fruit according to claim 1, is characterized in that checkout equipment is Agilent6890 gas chromatograph (being furnished with flame photometric detector (FPD)).
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110031355A (en) * | 2019-05-08 | 2019-07-19 | 青岛农业大学 | A method of evaluation and test forest trunk disease pesticide control lasting period and resistance of rainwater washing against ability |
| CN113203720A (en) * | 2021-06-15 | 2021-08-03 | 山西农业大学 | Method for detecting residual amount of dichlorvos in aquatic product by fluorescence analysis method and detection kit |
| CN114002360A (en) * | 2021-11-02 | 2022-02-01 | 江苏稻飘香米业股份有限公司 | Rice surface drug residue detection method |
-
2013
- 2013-08-30 CN CN2013104054222A patent/CN103439437A/en active Pending
Non-Patent Citations (4)
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| 王东群等: "气相色谱测定大米中有机磷农药残留量", 《粮油食品科技》 * |
| 王慧等: "气相色谱法测定韭菜中有机磷农药残留量", 《北京科技大学学报》 * |
| 蔡颖等: "蔬菜和水果中有机磷农药的双柱气相色谱测定法", 《环境与健康杂志》 * |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110031355A (en) * | 2019-05-08 | 2019-07-19 | 青岛农业大学 | A method of evaluation and test forest trunk disease pesticide control lasting period and resistance of rainwater washing against ability |
| CN110031355B (en) * | 2019-05-08 | 2022-01-28 | 青岛农业大学 | Method for evaluating duration and rain-wash resistance of forest branch disease control agent |
| CN113203720A (en) * | 2021-06-15 | 2021-08-03 | 山西农业大学 | Method for detecting residual amount of dichlorvos in aquatic product by fluorescence analysis method and detection kit |
| CN113203720B (en) * | 2021-06-15 | 2022-09-06 | 山西农业大学 | Method for detecting residual amount of dichlorvos in aquatic product by fluorescence analysis method and detection kit |
| CN114002360A (en) * | 2021-11-02 | 2022-02-01 | 江苏稻飘香米业股份有限公司 | Rice surface drug residue detection method |
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Application publication date: 20131211 |