CN110007024A - A kind of accurate quick On Detection of Organophosphorus Pesticide of vegetables - Google Patents
A kind of accurate quick On Detection of Organophosphorus Pesticide of vegetables Download PDFInfo
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- CN110007024A CN110007024A CN201910308455.2A CN201910308455A CN110007024A CN 110007024 A CN110007024 A CN 110007024A CN 201910308455 A CN201910308455 A CN 201910308455A CN 110007024 A CN110007024 A CN 110007024A
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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
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N2030/042—Standards
- G01N2030/047—Standards external
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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
- G01N2030/062—Preparation extracting sample from raw material
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Abstract
The invention discloses a kind of accurate quick On Detection of Organophosphorus Pesticide of vegetables, include the following steps: prepared by standard sample solution；Acetone, hexamethylene are uniformly mixed, eluent is obtained；Vegetables, silica are sent into grinder and are ground, grinding pressure 0.12-0.18MPa, milling time 20-40min obtain sample；Anhydrous sodium sulfate, sample, anhydrous sodium sulfate are sequentially added to syringe bottom, is compacted, is eluted using eluent and is then flowed out through syringe needle hole portion, eluent and putting is collected and is evaporated into ventilating kitchen dry, acetone solution and constant volume is added, obtains prepare liquid；It is analyzed with gas chromatographic detection instrument.The method of the present invention is simple, and detection sensitivity is high, the reproducibility with height, and detection speed is fast.
Description
Technical field
The present invention relates to organic phosphorus detection technique field more particularly to a kind of accurate quick detection of organic phosphorus pesticide of vegetables
Method.
Background technique
The development of modern agriculture makes agricultural product production be increasingly dependent on the allogenic materials such as pesticide, antibiotic and hormone.Its
In, pesticide dosage is high, and the unreasonable use of some pesticides keeps Residual Pesticides in Farm Produce exceeded, affects consumer
Edible safety, the routine testing and Risk Monitoring of pesticide residue become more and more important.As the improvement of people's living standards,
The food-safe problem of people is increasingly paid attention to, and it is organic to detect its as a kind of closely bound up food of living with people for vegetables
Phosphorus pesticide residue is significant, in addition, since vegetables are not easy to store for a long time, if detection cycle is too long, detection reproducibility
Difference, then Clinical significance of detecting substantially reduces.
Summary of the invention
Technical problems based on background technology, the invention proposes a kind of accurate quickly organophosphorus pesticide inspections of vegetables
Survey method, the method for the present invention is simple, and detection sensitivity is high, the reproducibility with height, and detection speed is fast.
A kind of accurate quick On Detection of Organophosphorus Pesticide of vegetables proposed by the present invention, includes the following steps:
S1, the preparation of standard sample solution:
S2,50-100 parts of acetone, 100-200 parts of hexamethylenes are uniformly mixed by weight, obtain eluent；
S3,100 portions of vegetables, 60-80 parts of silica are sent into grinder and are ground, grinding pressure 0.12-
0.18MPa, milling time 20-40min, obtains sample；
S4, to syringe bottom 2-4 parts of anhydrous sodium sulfates, 2-4 parts of samples, 2-4 parts of anhydrous sulphur are sequentially added by weight
Then sour sodium, compacting are flowed out through syringe needle hole portion using 10-14 parts of eluent elution, collect eluent and put Yu Tongfeng
It evaporates into dry in kitchen, acetone solution and constant volume is added, obtains prepare liquid；
S5, it is analyzed with gas chromatographic detection instrument.
Preferably, in S1, during the preparation of standard sample solution, organophosphorus pesticide is taken, it is dilute with n-hexane respectively
It is interpreted as the standard sample solution that mass concentration is 0.2mg/kg, 0.5mg/kg, 1mg/kg, 5mg/kg, 10mg/kg, 50mg/kg.
Preferably, in S1, the organophosphorus pesticide is thimet, parathion-methyl, malathion, DDVP, speed are gone out
Phosphorus, flolimat, ethoprop, Carbicron, Azodrin, thiometon, Rogor, propetamphos, diazinon, disulfoton, methyl pair
Sulphur phosphorus, fenifrothion, Entex, parathion, chlorfenviphos, quinalphos, Rilariol, Ravap, Profenofos, De-Green, three
Any one or more in azoles phosphorus, edifenphos, phenothiazide, azinphos-methyl, azinphos ethyl or Resistox.
Preferably, in S1, organophosphorus pesticide is thimet, parathion-methyl, malathion.
Preferably, in S2, acetone, hexamethylene weight ratio be 1-2:2-4.
Preferably, in S3, vegetables, silica weight ratio be 5:3-3.
Preferably, in S3, during grinding, grinding pressure 0.12-0.18MPa, milling time 20-
40min。
Preferably, in S5, wherein in gas chromatographic detection instrument:
Chromatographic column: 30m × 0.25mm × 0.25 μm, HP-5MS；
Input mode: Splitless injecting samples；Sample volume: 1 μ L；
Temperature programming: initial temperature is 100 DEG C, keeps 3min, is warming up to 190 DEG C with the speed of 14 DEG C/min, keeps
4min, then 200 DEG C are warming up to the speed of 12 DEG C/min, 5min is kept, then be warming up to 250 DEG C with the speed of 10 DEG C/min, protected
Hold 8min；
Carrier gas: helium, purity >=99.999%；Flow rate of carrier gas: 1.0mL/min；
Ionization mode: EI；Ionizing energy: 70eV；
Injector temperature: 230 DEG C；Transmission line temperature: 280 DEG C；Ion source temperature: 280 DEG C.
In the present invention, Silica Properties are stablized, and do not react with water, i.e., contact with water and do not generate silicic acid, compound with vegetables
Grinding, and in a certain range by control grinding pressure and milling time, vegetables can be made sufficiently to crush, not only grinding agent dioxy
The additional amount of SiClx is few, and shortens milling time, and can guarantee the accuracy and reliability of testing result；And acetone and hexamethylene
Alkane compounding is used as eluent, fabulous to the effect of extracting of sample, can farthest extract the organophosphorus pesticide in vegetables simultaneously
It takes out, using eluent in lessivation, organophosphorus pesticide can sufficiently be extracted, effectively improve extraction efficiency, regather
Prepare liquid, using acetone solution and constant volume after evaporating into and doing, dissolution degree is high, analyzes by gas chromatographic detection instrument, logical
Rationally control analysis condition is crossed, organophosphorus pesticide concentration range that can be detected is 0-100mg/L.
The present invention has high separation efficiency, selectivity height, high sensitivity, analysis fast speed, solvent and amount of samples few
The advantages of, and detection method of the invention also has the characteristics that rate of recovery height, favorable reproducibility, meets analysis and requires, is suitable for
The quick detection and analysis of Organo-phosphorus Pesticide Residues in Vegetables.
Specific embodiment
In the following, technical solution of the present invention is described in detail by specific embodiment.
Embodiment 1
A kind of accurate quick On Detection of Organophosphorus Pesticide of vegetables, includes the following steps:
S1, the preparation of standard sample solution: thimet, parathion-methyl, malathion are taken, is diluted to matter with n-hexane respectively
Measure the standard sample solution that concentration is 0.2mg/kg, 0.5mg/kg, 1mg/kg, 5mg/kg, 10mg/kg, 50mg/kg；
S2,55 parts of acetone, 105 parts of hexamethylenes are uniformly mixed by weight, obtain eluent；
S3,100 portions of vegetables, 60 parts of silica are sent into grinder and are ground, grinding pressure 0.13MPa is ground
Time consuming is 22min, obtains sample；
S4, to syringe bottom 2.3 parts of anhydrous sodium sulfates, 2.5 parts of samples, 2 parts of anhydrous slufuric acids are sequentially added by weight
Then sodium, compacting are flowed out through syringe needle hole portion using 10 parts of eluent elution, collect eluent and put and wave in ventilating kitchen
It is sent to dry, acetone solution and constant volume is added, obtains prepare liquid；
S5, it is analyzed with gas chromatographic detection instrument.
Wherein in gas chromatographic detection instrument:
Chromatographic column: 30m × 0.25mm × 0.25 μm, HP-5MS；
Input mode: Splitless injecting samples；Sample volume: 1 μ L；
Temperature programming: initial temperature is 100 DEG C, keeps 3min, is warming up to 190 DEG C with the speed of 14 DEG C/min, keeps
4min, then 200 DEG C are warming up to the speed of 12 DEG C/min, 5min is kept, then be warming up to 250 DEG C with the speed of 10 DEG C/min, protected
Hold 8min；
Carrier gas: helium, purity >=99.999%；Flow rate of carrier gas: 1.0mL/min；
Ionization mode: EI；Ionizing energy: 70eV；
Injector temperature: 230 DEG C；Transmission line temperature: 280 DEG C；Ion source temperature: 280 DEG C.
Embodiment 2
A kind of accurate quick On Detection of Organophosphorus Pesticide of vegetables, includes the following steps:
S1, the preparation of standard sample solution: thimet, parathion-methyl, malathion are taken, is diluted to matter with n-hexane respectively
Measure the standard sample solution that concentration is 0.2mg/kg, 0.5mg/kg, 1mg/kg, 5mg/kg, 10mg/kg, 50mg/kg；
S2,100 parts of acetone, 180 parts of hexamethylenes are uniformly mixed by weight, obtain eluent；
S3,100 portions of vegetables, 78 parts of silica are sent into grinder and are ground, grinding pressure 0.18MPa is ground
Time consuming is 40min, obtains sample；
S4, to syringe bottom 4 parts of anhydrous sodium sulfates, 3.8 parts of samples, 3.5 parts of anhydrous slufuric acids are sequentially added by weight
Then sodium, compacting are flowed out through syringe needle hole portion using 13.5 parts of eluent elution, collect eluent and put in ventilating kitchen
It evaporates into dry, acetone solution and constant volume is added, obtains prepare liquid；
S5, it is analyzed with gas chromatographic detection instrument.
Wherein in gas chromatographic detection instrument:
Chromatographic column: 30m × 0.25mm × 0.25 μm, HP-5MS；
Input mode: Splitless injecting samples；Sample volume: 1 μ L；
Temperature programming: initial temperature is 100 DEG C, keeps 3min, is warming up to 190 DEG C with the speed of 14 DEG C/min, keeps
4min, then 200 DEG C are warming up to the speed of 12 DEG C/min, 5min is kept, then be warming up to 250 DEG C with the speed of 10 DEG C/min, protected
Hold 8min；
Carrier gas: helium, purity >=99.999%；Flow rate of carrier gas: 1.0mL/min；
Ionization mode: EI；Ionizing energy: 70eV；
Injector temperature: 230 DEG C；Transmission line temperature: 280 DEG C；Ion source temperature: 280 DEG C.
It is embodiment 3
A kind of accurate quick On Detection of Organophosphorus Pesticide of vegetables, includes the following steps:
S1, the preparation of standard sample solution: thimet, parathion-methyl, malathion are taken, is diluted to matter with n-hexane respectively
Measure the standard sample solution that concentration is 0.2mg/kg, 0.5mg/kg, 1mg/kg, 5mg/kg, 10mg/kg, 50mg/kg；
S2,85 parts of acetone, 175 parts of hexamethylenes are uniformly mixed by weight, obtain eluent；
S3,100 portions of vegetables, 75 parts of silica are sent into grinder and are ground, grinding pressure 0.15MPa is ground
Time consuming is 35min, obtains sample；
S4, to syringe bottom 3 parts of anhydrous sodium sulfates, 3 parts of samples, 3 parts of anhydrous sodium sulfates are sequentially added by weight, pressed
It is real, it is then flowed out through syringe needle hole portion using 12 parts of eluents elution, collects eluent and put and evaporated into ventilating kitchen
It is dry, acetone solution and constant volume is added, obtains prepare liquid；
S5, it is analyzed with gas chromatographic detection instrument.
Wherein in gas chromatographic detection instrument:
Chromatographic column: 30m × 0.25mm × 0.25 μm, HP-5MS；
Input mode: Splitless injecting samples；Sample volume: 1 μ L；
Temperature programming: initial temperature is 100 DEG C, keeps 3min, is warming up to 190 DEG C with the speed of 14 DEG C/min, keeps
4min, then 200 DEG C are warming up to the speed of 12 DEG C/min, 5min is kept, then be warming up to 250 DEG C with the speed of 10 DEG C/min, protected
Hold 8min；
Carrier gas: helium, purity >=99.999%；Flow rate of carrier gas: 1.0mL/min；
Ionization mode: EI；Ionizing energy: 70eV；
Injector temperature: 230 DEG C；Transmission line temperature: 280 DEG C；Ion source temperature: 280 DEG C.
Embodiment 1-3 is detected with thimet, parathion-methyl, the configured standard solution in malathion, is detected
The rate of recovery is shown in Table 1, and the RSD for measuring sample is shown in Table 2:
The detection rate of recovery of 1 embodiment 1-3 Determination of Organic Phosphorus Pesticides in Vegetables of table
| Test item | Thimet/% | Parathion-methyl/% | Malathion/% |
| Embodiment 3 | 92.6 | 91.6 | 95.5 |
| Embodiment 4 | 97.6 | 93.8 | 91.4 |
| Embodiment 5 | 90.6 | 97.9 | 90.8 |
The RSD of 2 embodiment 1-3 of table measurement sample
| Test item | Thimet/% | Parathion-methyl/% | Malathion/% |
| Embodiment 3 | 1.1 | 1.2 | 1.8 |
| Embodiment 4 | 1.3 | 1.3 | 1.6 |
| Embodiment 5 | 0.8 | 1.8 | 1.2 |
From table 1, table 2 as can be seen that measuring the rate of recovery of thimet, parathion-methyl and malathion with the method for the present invention
Between 90.6-97.9%, relative standard deviation RSD illustrates this method accuracy with higher and reproducibility less than 1.8,
It can be used for quickly detecting Organo-phosphorus Pesticide Residues in Vegetables.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (8)
1. a kind of accurate quick On Detection of Organophosphorus Pesticide of vegetables, which comprises the steps of:
S1, the preparation of standard sample solution:
S2,50-100 parts of acetone, 100-200 parts of hexamethylenes are uniformly mixed by weight, obtain eluent；
S3,100 portions of vegetables, 60-80 parts of silica are sent into grinder and are ground, grinding pressure 0.12-
0.18MPa, milling time 20-40min, obtains sample；
S4, to syringe bottom 2-4 parts of anhydrous sodium sulfates, 2-4 parts of samples, 2-4 parts of anhydrous sodium sulfates are sequentially added by weight,
Then compacting is flowed out through syringe needle hole portion using 10-14 parts of eluent elution, collects eluent and put and wave in ventilating kitchen
It is sent to dry, acetone solution and constant volume is added, obtains prepare liquid；
S5, it is analyzed with gas chromatographic detection instrument.
2. the accurate quick On Detection of Organophosphorus Pesticide of vegetables according to claim 1, which is characterized in that in S1,
Standard sample solution preparation during, take organophosphorus pesticide, respectively with n-hexane be diluted to mass concentration be 0.2mg/kg,
The standard sample solution of 0.5mg/kg, 1mg/kg, 5mg/kg, 10mg/kg, 50mg/kg.
3. the accurate quick On Detection of Organophosphorus Pesticide of vegetables according to claim 2, which is characterized in that in S1,
The organophosphorus pesticide is thimet, parathion-methyl, malathion, DDVP, Menite, flolimat, ethoprop, hundred controls
It is phosphorus, Azodrin, thiometon, Rogor, propetamphos, diazinon, disulfoton, parathion-methyl, fenifrothion, Entex, right
Sulphur phosphorus, quinalphos, Rilariol, Ravap, Profenofos, De-Green, Hostathion, edifenphos, phenothiazide, protects cotton at chlorfenviphos
Any one or more in phosphorus, azinphos ethyl or Resistox.
4. the accurate quick On Detection of Organophosphorus Pesticide of vegetables according to claim 3, which is characterized in that in S1,
Organophosphorus pesticide includes thimet, parathion-methyl, malathion.
5. the accurate quick On Detection of Organophosphorus Pesticide of vegetables according to claim 1, which is characterized in that in S2,
Acetone, hexamethylene weight ratio be 1-2:2-4.
6. the accurate quick On Detection of Organophosphorus Pesticide of vegetables according to claim 1, which is characterized in that in S3,
Vegetables, silica weight ratio be 5:3-3.
7. the accurate quick On Detection of Organophosphorus Pesticide of vegetables according to claim 1, which is characterized in that in S3,
During grinding, grinding pressure 0.12-0.18MPa, milling time 20-40min.
8. the accurate quick On Detection of Organophosphorus Pesticide of vegetables according to claim 1-7, which is characterized in that
In S5, wherein in gas chromatographic detection instrument:
Chromatographic column: 30m × 0.25mm × 0.25 μm, HP-5MS；
Input mode: Splitless injecting samples；Sample volume: 1 μ L；
Temperature programming: initial temperature is 100 DEG C, keeps 3min, is warming up to 190 DEG C with the speed of 14 DEG C/min, keeps 4min, then
200 DEG C are warming up to the speed of 12 DEG C/min, 5min is kept, then be warming up to 250 DEG C with the speed of 10 DEG C/min, keeps 8min；
Carrier gas: helium, purity >=99.999%；Flow rate of carrier gas: 1.0mL/min；
Ionization mode: EI；Ionizing energy: 70eV；
Injector temperature: 230 DEG C；Transmission line temperature: 280 DEG C；Ion source temperature: 280 DEG C.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR102235092B1 (en) * | 2019-11-06 | 2021-04-01 | 강원대학교산학협력단 | Method for analyzing residual amount of disulfoton compound and its oxidation derivatives as pesticides |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR102235092B1 (en) * | 2019-11-06 | 2021-04-01 | 강원대학교산학협력단 | Method for analyzing residual amount of disulfoton compound and its oxidation derivatives as pesticides |
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