CN109668990A - The rapid assay methods of organophosphorus pesticide residue in a kind of vegetables - Google Patents
The rapid assay methods of organophosphorus pesticide residue in a kind of vegetables Download PDFInfo
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- CN109668990A CN109668990A CN201910163767.9A CN201910163767A CN109668990A CN 109668990 A CN109668990 A CN 109668990A CN 201910163767 A CN201910163767 A CN 201910163767A CN 109668990 A CN109668990 A CN 109668990A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/60—Construction of the column
- G01N30/6052—Construction of the column body
- G01N30/6073—Construction of the column body in open tubular form
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Abstract
The invention discloses a kind of rapid assay methods of organophosphorus pesticide residue in vegetables, the following steps are included: (1) sample extraction and purification: taking 10-20g sample, 50-200mL sample extracting solution is added, the mixing of 10-20g sodium chloride is added after concussion filtering, acetone is precipitated, it is concentrated after drawing acetone, is finally settled to 1mL with acetone and obtains test sample；(2) it detects: the sample prepared in step (1) being detected using gas chromatograph.The rapid assay methods of organophosphorus pesticide residue in a kind of vegetables provided by the invention, have selected the chromatographic condition of measurement, so that organophosphorus pesticide hybrid standard liquid has obtained good separation, entire separation process time-consuming is short, the peak shape and separating degree of chromatographic peak are all fine, it is qualitative with retention time progress by testing result, it is compared quantitatively with the peak area of sample or peak height with the peak area of standard sample or peak height.
Description
Technical field
The present invention relates to field of pesticide detection, and in particular to the quick measurement side of organophosphorus pesticide residue in a kind of vegetables
Method.
Background technique
The type of pesticide is varied, and is increasing every year new varieties, so far, in the agriculture of countries in the world registration
Drug kind is more than 1500 kinds existing, wherein there are commonly more than 500.Mineral sources, chemical synthesis and biological source three can be by sources divided into
Major class；Inorganic, organic, antibiotic and biological pesticide can be divided by its chemical structure, wherein organic include organic phosphates,
Organochlorine class, carbamates, pyrethroid and organic metal class pesticide etc.；Desinsection can be divided by main controlling object
Agent, acaricide, fungicide, rat poison, nematicide, herbicide and plant growth regulator etc..Pesticide residue refers to that pesticide makes
The general name of pesticide substance in organism, agricultural and sideline product and environment, toxic metabolite, degradation product and impurity is remained in after, it is residual
The quantity stayed is known as residual quantity.Pesticide residue is primarily referred to as the residual quantity of pesticide substance and has than substance poison under normal circumstances
Property higher or suitable toxicity degradation product residual quantity, and photostability possessed by the size of persticide residue and the pesticide,
The factors such as chemical stability, microbial degradation stability are related.
With living standards of the people raising and environmental protection, health perception enhancing, people more focuses on vegetables health with
Safety.Food especially pesticide residues in vegetables chemicals contamination causes acute poisoning event to appear in the newspapers repeatly to lead, seriously affected the people in recent years
The life and health of the masses, this social concern have caused extensive concern.But pesticide generates the chronic hazard of human body
Physiological change is usually ignored because being easy without manifest symptom, causes that some properties are relatively stable, have savings property malicious again people
Harmful chemical pesticide polluted natural environment, and by biological concentration and food chain lock, cause them in animal and plant body, very
To storing up people is intracorporal, there is the pollution problem of pesticide today.Due to vegetables by the source of pesticide and environmental pollution often
Unclear, furthermore pesticide has homologue, isomers, degradation product and metabolin etc., the physical chemistry of different type pesticide mostly
Matter is not again identical, and component to be measured also becomes increasingly complex, and which increase the difficulty of pesticide residue analysis.
Summary of the invention
The purpose of the present invention is to provide a kind of rapid assay methods of organophosphorus pesticide residue in vegetables, can be to vegetable
Organophosphorus pesticide residue fast qualitative and quantitative detection in dish.
To achieve the above object, technical solution provided by the invention is as follows:
The rapid assay methods of organophosphorus pesticide residue in a kind of vegetables, comprising the following steps:
(1) sample extraction and purification: taking 10-20g sample, and 50-200mL sample extracting solution is added, is added after concussion filtering
Acetone is precipitated in the mixing of 10-20g sodium chloride, is concentrated after drawing acetone, is finally settled to 1mL with acetone and obtains test sample；
(2) it detects: the sample prepared in step (1) being detected using gas chromatograph；
The condition of gas-chromatography is as follows:
Chromatographic column: 30m × 0.32mm × 0.20 μm DB-1701 quartz elastic capillary tube chromatographic column or SPB-5 30m ×
0.25mm × 0.25 μm quartz elastic capillary tube chromatographic column；
Gas flow rate: high pure nitrogen (> 99.999%) is carrier gas, flow rate of carrier gas: 2mL/min；Make-up gas 30-50mL/
min；Hydrogen 80-100mL/min；Air 70-90mL/min；
Temperature of vaporization chamber: 200-250 DEG C；Detector temperature: 200-250 DEG C；Column temperature program: initial temperature 50-200
DEG C, 185 DEG C are risen to 10-20 DEG C/min, constant temperature 5-15min.
Further, the sample extracting solution is one or both of acetone or acetonitrile.
Further, the concussion time is 20-40min.
Further, the step of addition sodium chloride mixes includes: concussion 1-3min, stands 5-15min.
It further, include: accurate suction using the configuration method of gas-chromatography test Plays solution in the step (2)
It takes organic phosphorus standard to be detected using solution in 50mL volumetric flask, with acetone constant volume, draws this standard respectively and use solution
1mL, 2mL, 4mL, 6mL, 8mL, 10mL are settled to 10mL with acetone, and being configured to concentration is respectively 0.02 μ g/mL, 0.04 μ g/
ML, 0.08 μ g/mL, 0.12 μ g/mL, 0.16 μ g/mL, the standard solution of 0.20 μ g/mL.
Further, the chromatographic column is 30m × 0.32mm × 0.20 μm DB-1701 quartz elastic capillary tube chromatographic column.
Further, the column temperature program specifically includes: 80 DEG C of initial temperature, rising to 185 DEG C with 15 DEG C/min, constant temperature
10min。
The present invention has the advantages that
Sample containing organophosphorus pesticide, through chromatography post separation, burns after extraction, purification, concentration on hydrogen-rich flame,
Wavelength is radiated as the characteristic light of 526nm with form of chips, after this light is selected by optical filter, is received by photomultiplier tube,
It is converted into electric signal, is recorded after micro current amplifier amplifies, it is qualitative with retention time, with the peak area or peak of sample
Height is compared quantitative with the peak area of standard sample or peak height；The present invention has selected the chromatographic condition of measurement, so that organic phosphorus
Pestsides synthesis titer has obtained good separation, and entire separation process time-consuming is short, and the peak shape and separating degree of chromatographic peak are all fine.
Specific embodiment
The technical scheme of the present invention will be further described combined with specific embodiments below, but those skilled in the art will
It will be appreciated that how embodiment what follows is merely to illustrate using the present invention, and it is not construed as limiting the scope of the invention.Base
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts it is all its
His embodiment, shall fall within the protection scope of the present invention.
Embodiment
(1) sample extraction and purification:
20g sample is taken, 50mL water and 100mL acetone is added, 15g sodium chloride is added after concussion 30min filtering and shakes 2min,
10min is stood, is come so that acetone is salted out from water phase, is filtered by anhydrous sodium sulfate funnel to concentrate bottle after drawing acetone
In, then with 40mL acetone, washing funnel and anhydrous sodium sulfate, cleaning solution are also incorporated into concentrate bottle by several times, are concentrated with rotary evaporator
It is done to close, is finally settled to 1mL with acetone and obtains test sample；
The configuration method of standard solution:
Accurately drawing organic phosphorus standard to be detected uses solution in 50mL volumetric flask, with acetone constant volume, draws this respectively
Standard uses solution 1mL, 2mL, 4mL, 6mL, 8mL, 10mL, is settled to 10mL with acetone, being configured to concentration is respectively 0.02 μ g/
ML, 0.04 μ g/mL, 0.08 μ g/mL, 0.12 μ g/mL, 0.16 μ g/mL, the standard solution of 0.20 μ g/mL；
(2) it detects:
The sample prepared in step (1) is detected using gas chromatograph；
The condition of gas-chromatography is as follows:
Chromatographic column: 30m × 0.32mm × 0.20 μm DB-1701 quartz elastic capillary tube chromatographic column；
Gas flow rate: high pure nitrogen (> 99.999%) is carrier gas, flow rate of carrier gas: 2mL/min；Make-up gas 40mL/min；Hydrogen
Gas 90mL/min；Air 80mL/min；
Temperature of vaporization chamber: 250 DEG C；Detector temperature: 250 DEG C；Column temperature program: 80 DEG C of initial temperature, with 15 DEG C/min
185 DEG C are risen to, constant temperature 10min.
Chromatography: measuring in 1 μ L mark solution and sample scavenging solution injection gas chromatograph, qualitative with retention time,
It is quantitative with sample peak height or peak area and standard comparing.
As a result it calculates: X=W × V × 1/M
Wherein, content organic phosphorus in X- sample, mg/Kg；
W- injects content organic phosphorus in sample, μ g/mL；
Constant volume, mL is concentrated in V- sample；
The comparable sample mass of constant volume institute, g is concentrated in M- sample.
Testing result shows that organophosphorus pesticide hybrid standard liquid has obtained good separation under selected chromatographic condition,
Entire separation process time-consuming is short, and the peak shape and separating degree of chromatographic peak are all fine.
This rapid assay methods are as shown in the table to the result of 153 kinds of organophosphorus insecticide abilities of screening:
By taking three kinds of spinach, tomato and celery vegetables as an example.
Screening for above-mentioned 153 kinds of organophosphorus insecticides, as the result is shown this method can screening pesticide quantity at least
It is 139 kinds, accounts for toatl proportion 90.9%, shows this method to the high sensitivity of organophosphorus insecticide in vegetables, screening ability
It is relatively strong.
Finally, it should be noted that above embodiments are only to illustrate the present invention and not limit technology described in the invention
Scheme；Those skilled in the art should understand that still can modify to the present invention or equivalent replacement；And all are not
It is detached from the technical solution and its improvement of the spirit and scope of the present invention, should all be covered within the scope of the claims of the present invention.
Claims (7)
1. the rapid assay methods of organophosphorus pesticide residue in a kind of vegetables, which is characterized in that
The following steps are included:
(1) sample extraction and purification: taking 10-20g sample, and 50-200mL sample extracting solution is added, 10- is added after concussion filtering
Acetone is precipitated in the mixing of 20g sodium chloride, is concentrated after drawing acetone, is finally settled to 1mL with acetone and obtains test sample；
(2) it detects: the sample prepared in step (1) being detected using gas chromatograph；
The condition of gas-chromatography is as follows:
Chromatographic column: 30m × 0.32mm × 0.20 μm DB-1701 quartz elastic capillary tube chromatographic column or SPB-5 30m ×
0.25mm × 0.25 μm quartz elastic capillary tube chromatographic column；
Gas flow rate: high pure nitrogen (> 99.999%) is carrier gas, flow rate of carrier gas: 2mL/min；Make-up gas 30-50mL/min；Hydrogen
Gas 80-100mL/min；Air 70-90mL/min；
Temperature of vaporization chamber: 200-250 DEG C；Detector temperature: 200-250 DEG C；Column temperature program: 50-200 DEG C of initial temperature, with
10-20 DEG C/min rises to 185 DEG C, constant temperature 5-15min.
2. the method according to claim 1, wherein the sample extracting solution be one of acetone or acetonitrile or
Two kinds.
3. the method according to claim 1, wherein the concussion time is 20-40min.
4. the method according to claim 1, wherein the addition sodium chloride includes: concussion 1- the step of mixing
3min stands 5-15min.
5. the method according to claim 1, wherein testing Plays using gas-chromatography in the step (2)
The configuration method of solution includes: accurately to draw organic phosphorus standard to be detected using solution in 50mL volumetric flask, with acetone constant volume,
This standard is drawn respectively using solution 1mL, 2mL, 4mL, 6mL, 8mL, 10mL, is settled to 10mL with acetone, is configured to concentration point
Not Wei the μ of 0.02 μ g/mL, 0.04 μ g/mL, 0.08 g/mL, 0.12 μ g/mL, 0.16 μ g/mL, the standard solution of 0.20 μ g/mL.
6. the method according to claim 1, wherein the chromatographic column be DB-1701 30m × 0.32mm ×
0.20 μm of quartz elastic capillary tube chromatographic column.
7. the method according to claim 1, wherein the column temperature program specifically includes: 80 DEG C of initial temperature,
185 DEG C are risen to 15 DEG C/min, constant temperature 10min.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110361477A (en) * | 2019-08-13 | 2019-10-22 | 深圳市深大检测有限公司 | The measurement of organic phosphorus pesticide multi-residue in vegetables and fruit |
| CN112834648A (en) * | 2020-12-31 | 2021-05-25 | 镇江华大检测有限公司 | Method for detecting pesticide residues in vegetables and fruits |
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| US3547588A (en) * | 1968-01-12 | 1970-12-15 | Sumitomo Chemical Co | Gaschromatographic determination of minute amount of organophosphorus compounds |
| CN101799460A (en) * | 2010-04-28 | 2010-08-11 | 中国烟草总公司郑州烟草研究院 | Method for detecting organophosphorus pesticide residue in tobacco |
| CN102121928A (en) * | 2010-12-20 | 2011-07-13 | 天津市农业科学院中心实验室 | Method for processing onion sample containing several pesticide residues before determination |
| WO2013068026A1 (en) * | 2011-11-07 | 2013-05-16 | Tehran University Of Medical Sciences (Tums), Faculty Of Environmental University Of Tehran | Development of a new coating for sorptive extraction by stir bars |
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| US3547588A (en) * | 1968-01-12 | 1970-12-15 | Sumitomo Chemical Co | Gaschromatographic determination of minute amount of organophosphorus compounds |
| CN101799460A (en) * | 2010-04-28 | 2010-08-11 | 中国烟草总公司郑州烟草研究院 | Method for detecting organophosphorus pesticide residue in tobacco |
| CN102121928A (en) * | 2010-12-20 | 2011-07-13 | 天津市农业科学院中心实验室 | Method for processing onion sample containing several pesticide residues before determination |
| WO2013068026A1 (en) * | 2011-11-07 | 2013-05-16 | Tehran University Of Medical Sciences (Tums), Faculty Of Environmental University Of Tehran | Development of a new coating for sorptive extraction by stir bars |
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| CN103884788A (en) * | 2014-02-26 | 2014-06-25 | 华中农业大学 | Method for detecting pesticide residues in tea by using gas chromatograph-mass spectrometry |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110361477A (en) * | 2019-08-13 | 2019-10-22 | 深圳市深大检测有限公司 | The measurement of organic phosphorus pesticide multi-residue in vegetables and fruit |
| CN110361477B (en) * | 2019-08-13 | 2021-12-28 | 深圳市深大检测有限公司 | Determination of organophosphorus pesticide residue in vegetables and fruits |
| CN112834648A (en) * | 2020-12-31 | 2021-05-25 | 镇江华大检测有限公司 | Method for detecting pesticide residues in vegetables and fruits |
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Application publication date: 20190423 |