CN108414639A - A kind of rapid detection method of Pesticide Residues object - Google Patents
A kind of rapid detection method of Pesticide Residues object Download PDFInfo
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- CN108414639A CN108414639A CN201810257580.0A CN201810257580A CN108414639A CN 108414639 A CN108414639 A CN 108414639A CN 201810257580 A CN201810257580 A CN 201810257580A CN 108414639 A CN108414639 A CN 108414639A
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- G—PHYSICS
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- 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
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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
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Abstract
The invention discloses a kind of rapid detection methods of Pesticide Residues object, include the following steps：（1）Food pre-treatment；（2）By the GC MS quantitative analyses of pre-treatment good sample, the residual content of food middle peasant is obtained.The rapid detection method high sensitivity of the Pesticide Residues object of the present invention, stability is high, it is easy to operate, with higher precision and repeatability, the range of linearity is preferable, and sample recovery rate experiment meets the requirements, and measurement result is accurate and reliable, it is efficient, it disclosure satisfy that the needs that Pesticide Residues quickly detect.
Description
Technical field
The present invention relates to a kind of detection method, the rapid detection method of specifically a kind of Pesticide Residues object.
Background technology
Pesticide can be used for killing the biology of insect, fungi and the growth of other damages to crops.The pesticide used earliest has drop
DDT, six six six etc., they can largely eliminate pest.But their stability is good, can long-term existence in the environment, and planted dynamic
It constantly accumulates in object and human body, is eliminated thus.It used organophosphorus pesticide, such as DDVP instead later, and substituted initial pesticide.So
And their toxicity is too big, it is very big to the harm of people and animals.In recent years, the pesticide of a collection of high-efficiency low-toxicity occurs, and present people are
Have found the pesticide with specificity, i.e. steroids pesticide.However, improving regardless of pesticide has, belong to chemicals scope after all more,
Environment can be impacted, health is impacted.Because for food security, need to carry out pesticide residue to food
Detection.
Currently, the common detection methods of pesticide residue have：Thin-layered chromatography, high performance liquid chromatography, surpasses gas chromatography
Critical fluids chromatography etc..Wherein, Instrumental Analysis detection method precision highest, but its detection process is complicated, detection time is long.Together
When, is detected cumbersome, and efficiency is low, and reviewer contacts poisonous and harmful substance chance and increases, and damages quality inspection personnel health.
Biochemistry detection technology is quickly grown, but early investment is big, experiment condition is harsh.Therefore, the present invention provides a kind of food middle peasant
The rapid detection method of medicine residue.
Invention content
The purpose of the present invention is to provide a kind of rapid detection methods of Pesticide Residues object, to solve above-mentioned background
The problem of being proposed in technology.
To achieve the above object, the present invention provides the following technical solutions：
A kind of rapid detection method of Pesticide Residues object, includes the following steps：
（1）Food pre-treatment：1.0g test samples are weighed, is placed at 50-75 DEG C and dries, the 200-400 mesh that then pulverizes and sieves sieve,
Ethanol solution 3-5mL, a concentration of 0.01-0.1mol/L citric acid solutions 5-8mL and the concentration that mass fraction is 40-50% is added
For 0.01-0.03mol/L acetum 15-30mL, it is ultrasonically treated 10-15min, filtering, then with 0.01-0.03mol/L acetic acid
10-25mL points of 3 washing residues of solution, solution adjust pH to 6.0-8.0 with 1-2mol/L calcium hydroxide solutions, Boratex are added
1-5mg, sodium carbonate 4-6mg, anhydrous zinc sulfate 0.1-0.3mg and acetonitrile 10-20mL, react 25- in 55-75 DEG C of water-bath
After taking out cooling, 30-50mL chloroform extractions, layering is added in 40min, and extraction is repeated twice, and combining extraction liquid is through anhydrous sulphur
Sour sodium drying, is spin-dried for, to be tested with methanol constant volume to 1.0mL；
（2）By pre-treatment good sample GC-MS quantitative analyses, the residual content of food middle peasant is obtained.
As a further solution of the present invention：Step（2）Determination condition is as follows：1. gas phase condition：Chromatographic column is HP-5 stones
English capillary column, wherein column length 30m, a diameter of 250 μm, film thickness is 0.25 μm；Chromatogram column temperature：45 DEG C of holding 1min, so
Afterwards with 10-20 DEG C/min temperature programmings to 150 DEG C, then with 2-3 DEG C/min it is warming up to 295-320 DEG C, and keeps 10min；Sample introduction
Mouth temperature：250℃；2. Mass Spectrometry Conditions：Ion source temperature：230℃；Level four bars temperature：150℃；Electron bombardment ionization source voltage：
70eV；GC-MS interface temperatures：280℃；3. monitoring mode：Full scan/Salbutamol Selected Ion Monitoring simultaneously examine by acquisition mode, full scan
Measured ion range：60-350amu.
As a further solution of the present invention：Step（1）Middle ethanol solution mass fraction is 45%.
As a further solution of the present invention：Step（1）Middle a concentration of 0.05mol/L of citric acid solution.
As a further solution of the present invention：Step（1）Middle a concentration of 0.02mol/L of acetum.
As a further solution of the present invention：Step（1）Middle addition Boratex 2mg, sodium carbonate 5mg, anhydrous zinc sulfate
0.2mg and acetonitrile 16mL.
Compared with prior art, the beneficial effects of the invention are as follows：
The rapid detection method high sensitivity of the Pesticide Residues object of the present invention, stability is high, easy to operate, has higher
Precision and repeatability, the range of linearity is preferable, sample recovery rate experiment meets the requirements, measurement result is accurate and reliable, efficiency
Height disclosure satisfy that the needs that Pesticide Residues quickly detect.
Specific implementation mode
The technical solution of this patent is described in more detail With reference to embodiment.
Embodiment 1
A kind of rapid detection method of Pesticide Residues object, includes the following steps：（1）Food pre-treatment：Weigh 1.0g surveys
Test agent, is placed at 50 DEG C and dries, and ethanol solution 3mL, the concentration that mass fraction is 40% is added in 200 mesh that then pulverize and sieve sieve
For 0.01mol/L citric acid solutions 5mL and a concentration of 0.01mol/L acetums 15mL, it is ultrasonically treated 10min, is filtered, then
With 10mL points of 3 washing residues of 0.01mol/L acetums, solution adjusts pH to 6.0 with 1mol/L calcium hydroxide solutions, is added
Boratex 1mg, sodium carbonate 4mg, anhydrous zinc sulfate 0.1mg and acetonitrile 10mL react 25min in 55 DEG C of water-baths, take out cooling
Afterwards, 30mL chloroform extractions, layering is added, extraction is repeated twice, and combining extraction liquid is dried over anhydrous sodium sulfate, and is spin-dried for, and is used
Methanol constant volume is to be tested to 1.0mL；（2）By pre-treatment good sample GC-MS quantitative analyses, obtain that food middle peasant is residual to be contained
Amount.Step（2）Determination condition is as follows：1. gas phase condition：Chromatographic column is HP-5 quartz capillary columns, wherein column length 30m, directly
Diameter is 250 μm, and film thickness is 0.25 μm；Chromatogram column temperature：45 DEG C of holding 1min, then with 10 DEG C/min temperature programmings to 150 DEG C,
295 DEG C are warming up to 2 DEG C/min again, and keeps 10min；Injector temperature：250℃；2. Mass Spectrometry Conditions：Ion source temperature：230
℃；Level four bars temperature：150℃；Electron bombardment ionization source voltage：70eV；GC-MS interface temperatures：280℃；3. monitoring mode：It sweeps entirely
Retouch/acquisition mode, full scan detect ion range to Salbutamol Selected Ion Monitoring simultaneously：60-350amu.
Embodiment 2
A kind of rapid detection method of Pesticide Residues object, includes the following steps：（1）Food pre-treatment：Weigh 1.0g surveys
Test agent, is placed at 75 DEG C and dries, and ethanol solution 5mL, the concentration that mass fraction is 50% is added in 400 mesh that then pulverize and sieve sieve
For 0.1mol/L citric acid solutions 8mL and a concentration of 0.03mol/L acetums 30mL, it is ultrasonically treated 15min, filtering, then use
25mL points of 3 washing residues of 0.03mol/L acetums, solution adjust pH to 8.0 with 2mol/L calcium hydroxide solutions, boron are added
Sour sodium 5mg, sodium carbonate 6mg, anhydrous zinc sulfate 0.3mg and acetonitrile 20mL react 40min in 75 DEG C of water-baths, after taking out cooling,
50mL chloroform extractions, layering is added, extraction is repeated twice, and combining extraction liquid is dried over anhydrous sodium sulfate, and is spin-dried for, and methanol is used
It is settled to 1.0mL, it is to be tested；（2）By pre-treatment good sample GC-MS quantitative analyses, the residual content of food middle peasant is obtained.Step
Suddenly（2）Determination condition is as follows：1. gas phase condition：Chromatographic column is HP-5 quartz capillary columns, wherein column length 30m, it is a diameter of
250 μm, film thickness is 0.25 μm；Chromatogram column temperature：45 DEG C of holding 1min, then with 20 DEG C/min temperature programmings to 150 DEG C, then with
3 DEG C/min is warming up to 320 DEG C, and keeps 10min；Injector temperature：250℃；2. Mass Spectrometry Conditions：Ion source temperature：230℃；
Level four bars temperature：150℃；Electron bombardment ionization source voltage：70eV；GC-MS interface temperatures：280℃；3. monitoring mode：Full scan/choosing
Ion monitoring acquisition mode simultaneously is selected, full scan detects ion range：60-350amu.
Embodiment 3
A kind of rapid detection method of Pesticide Residues object, includes the following steps：（1）Food pre-treatment：Weigh 1.0g surveys
Test agent, is placed at 65 DEG C and dries, and ethanol solution 4mL, the concentration that mass fraction is 45% is added in 300 mesh that then pulverize and sieve sieve
For 0.05mol/L citric acid solutions 6mL and a concentration of 0.02mol/L acetums 22mL, it is ultrasonically treated 13min, is filtered, then
With 15mL points of 3 washing residues of 0.02mol/L acetums, solution adjusts pH to 7.0 with 1.5mol/L calcium hydroxide solutions, adds
Enter Boratex 2mg, sodium carbonate 5mg, anhydrous zinc sulfate 0.2mg and acetonitrile 16mL, 30min is reacted in 65 DEG C of water-baths, takes out cold
But after, 40mL chloroform extractions, layering is added, extraction is repeated twice, and combining extraction liquid is dried over anhydrous sodium sulfate, and is spin-dried for,
It is to be tested with methanol constant volume to 1.0mL；（2）By pre-treatment good sample GC-MS quantitative analyses, it is residual to obtain food middle peasant
Content.Step（2）Determination condition is as follows：1. gas phase condition：Chromatographic column is HP-5 quartz capillary columns, wherein column length 30m,
A diameter of 250 μm, film thickness is 0.25 μm；Chromatogram column temperature：45 DEG C of holding 1min, then with 16 DEG C/min temperature programmings to 150
DEG C, then 305 DEG C are warming up to 2.5 DEG C/min, and keep 10min；Injector temperature：250℃；2. Mass Spectrometry Conditions：Ion source temperature
Degree：230℃；Level four bars temperature：150℃；Electron bombardment ionization source voltage：70eV；GC-MS interface temperatures：280℃；3. monitoring mode：
Acquisition mode, full scan detect ion range to full scan/Salbutamol Selected Ion Monitoring simultaneously：60-350amu.
Embodiment 4
A kind of rapid detection method of Pesticide Residues object, includes the following steps：（1）Food pre-treatment：Weigh 1.0g surveys
Test agent, is placed at 70 DEG C and dries, and the ethanol solution 4.5mL, dense that mass fraction is 48% is added in 350 mesh that then pulverize and sieve sieve
Degree is 0.03mol/L citric acid solutions 7mL and a concentration of 0.015mol/L acetums 26mL, is ultrasonically treated 12min, is filtered,
Use 0.025mol/L acetums 20mL points of 3 washing residues again, solution 1.7mol/L calcium hydroxide solutions adjust pH to
6.8, Boratex 4mg, sodium carbonate 4.2mg, anhydrous zinc sulfate 0.25mg and acetonitrile 13mL is added, is reacted in 60 DEG C of water-baths
After taking out cooling, 33mL chloroform extractions, layering is added in 34min, and extraction is repeated twice, and combining extraction liquid is through anhydrous slufuric acid
Sodium is dried, and is spin-dried for, to be tested with methanol constant volume to 1.0mL；（2）By pre-treatment good sample GC-MS quantitative analyses, obtain
The residual content of food middle peasant.Step（2）Determination condition is as follows：1. gas phase condition：Chromatographic column is HP-5 quartz capillary columns,
In, column length 30m, a diameter of 250 μm, film thickness is 0.25 μm；Chromatogram column temperature：45 DEG C of holding 1min, then with 12 DEG C/min
Temperature programming is warming up to 310 DEG C to 150 DEG C, then with 2.2 DEG C/min, and keeps 10min；Injector temperature：250℃；2. mass spectrum
Condition：Ion source temperature：230℃；Level four bars temperature：150℃；Electron bombardment ionization source voltage：70eV；GC-MS interface temperatures：280
℃；3. monitoring mode：Acquisition mode, full scan detect ion range to full scan/Salbutamol Selected Ion Monitoring simultaneously：60-350amu.
The present invention has the following advantages：High sensitivity, stability is high, easy to operate, has higher precision and repetition
Property, the range of linearity is preferable, and sample recovery rate experiment meets the requirements, and measurement result is accurate and reliable, efficient, disclosure satisfy that food
The needs of middle Fast Determination of Pesticide Residue.
The better embodiment of this patent is explained in detail above, but this patent is not limited to above-mentioned embodiment party
Formula, one skilled in the relevant art within the scope of knowledge, can also be under the premise of not departing from this patent objective
Various changes can be made.
Claims (6)
1. a kind of rapid detection method of Pesticide Residues object, which is characterized in that include the following steps：
（1）Food pre-treatment：1.0g test samples are weighed, is placed at 50-75 DEG C and dries, the 200-400 mesh that then pulverizes and sieves sieve,
Ethanol solution 3-5mL, a concentration of 0.01-0.1mol/L citric acid solutions 5-8mL and the concentration that mass fraction is 40-50% is added
For 0.01-0.03mol/L acetum 15-30mL, it is ultrasonically treated 10-15min, filtering, then with 0.01-0.03mol/L acetic acid
10-25mL points of 3 washing residues of solution, solution adjust pH to 6.0-8.0 with 1-2mol/L calcium hydroxide solutions, Boratex are added
1-5mg, sodium carbonate 4-6mg, anhydrous zinc sulfate 0.1-0.3mg and acetonitrile 10-20mL, react 25- in 55-75 DEG C of water-bath
After taking out cooling, 30-50mL chloroform extractions, layering is added in 40min, and extraction is repeated twice, and combining extraction liquid is through anhydrous sulphur
Sour sodium drying, is spin-dried for, to be tested with methanol constant volume to 1.0mL；
（2）By pre-treatment good sample GC-MS quantitative analyses, the residual content of food middle peasant is obtained.
2. the rapid detection method of Pesticide Residues object according to claim 1, which is characterized in that step（2）It surveys
Fixed condition is as follows：1. gas phase condition：Chromatographic column is HP-5 quartz capillary columns, wherein column length 30m, a diameter of 250 μm, and film
Thickness is 0.25 μm；Chromatogram column temperature：45 DEG C of holding 1min, then with 10-20 DEG C/min temperature programmings to 150 DEG C, then with 2-3
DEG C/min is warming up to 295-320 DEG C, and keeps 10min；Injector temperature：250℃；2. Mass Spectrometry Conditions：Ion source temperature：230
℃；Level four bars temperature：150℃；Electron bombardment ionization source voltage：70eV；GC-MS interface temperatures：280℃；3. monitoring mode：It sweeps entirely
Retouch/acquisition mode, full scan detect ion range to Salbutamol Selected Ion Monitoring simultaneously：60-350amu.
3. the rapid detection method of Pesticide Residues object according to claim 1, which is characterized in that step（1）In
Ethanol solution mass fraction is 45%.
4. the rapid detection method of Pesticide Residues object according to claim 1, which is characterized in that step（1）In
A concentration of 0.05mol/L of citric acid solution.
5. the rapid detection method of Pesticide Residues object according to claim 1, which is characterized in that step（1）In
A concentration of 0.02mol/L of acetum.
6. the rapid detection method of Pesticide Residues object according to claim 1, which is characterized in that step（1）In
Boratex 2mg, sodium carbonate 5mg, anhydrous zinc sulfate 0.2mg and acetonitrile 16mL is added.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113624889A (en) * | 2021-08-26 | 2021-11-09 | 衢州市食品药品检验研究院(衢州市医疗器械质量监督检验所) | Method for detecting 26 pesticide residues in royal jelly |
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| CN105717224A (en) * | 2016-01-30 | 2016-06-29 | 郭庆龙 | GC-EI-MS method for rapidly determining residual aminobenzene pyrazolone amount |
| CN105675604A (en) * | 2016-03-31 | 2016-06-15 | 山东五洲检测有限公司 | Method for detecting antibiotic residues in milk |
| CN105891200A (en) * | 2016-03-31 | 2016-08-24 | 山东五洲检测有限公司 | Method for detecting organophosphorus pesticide residues in vegetables |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113624889A (en) * | 2021-08-26 | 2021-11-09 | 衢州市食品药品检验研究院(衢州市医疗器械质量监督检验所) | Method for detecting 26 pesticide residues in royal jelly |
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