CN107831257A - A kind of organophosphorus residue quantity measuring method - Google Patents
A kind of organophosphorus residue quantity measuring method Download PDFInfo
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- CN107831257A CN107831257A CN201711018326.7A CN201711018326A CN107831257A CN 107831257 A CN107831257 A CN 107831257A CN 201711018326 A CN201711018326 A CN 201711018326A CN 107831257 A CN107831257 A CN 107831257A
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- organophosphorus
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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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
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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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
- G01N2030/884—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample organic compounds
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Abstract
The invention discloses a kind of organophosphorus residue quantity measuring method, comprise the steps of, A, sample preparation, extract, B, chromatogram collection, C, the chromatogram gathered to step B are analyzed, result of calculation.The organophosphorus pesticide data that organophosphorus residue quantity measuring method of the present invention is treated by chromatogram sampling analysis method in detectable substance carry out quick, sensitive, accurate, easy extraction and analysis, disclosure satisfy that farming residual analysis regulation and require.
Description
Technical field
The present invention relates to a kind of detection method, specifically a kind of organophosphorus residue quantity measuring method.
Background technology
The life of vegetables and people are closely bound up, and the nutriment of vegetables mainly includes mineral matter, vitamin, fiber etc.,
The content of these materials is higher, and the nutritive value of vegetables is also higher.In addition, the content of the moisture and dietary fiber in vegetables is also
Important Nutrition quality indicator.The nutrient of vegetables can not be underestimated, and nineteen ninety, world food and agricultural organization counted dimension life needed by human
The 90% of plain C, the 60% of vitamin A is all from vegetables, it is seen that contribution of the vegetables to human health it is huge.In addition, in vegetables
Also various plants chemical substance is the putative composition beneficial to health, as carotenoid, two propen compounds,
Methyl sulfide compound etc., many vegetables also containing unique trace element, have special health-care efficacy, such as tomato to human body
In lycopene, prostaglandin in onion etc..
Vegetables are in planting process, in order to prevent and treat pest and disease damage, are required to spray insecticide, wherein organophosphorus pesticide is because of kind
The reasons such as more, drug effect is high, purposes is wide are widely used in a variety of applications.A large amount of use of organophosphorus pesticide not only causes serious ring
Border is polluted, and injures the health of the mankind.The analysis method of detection organophosphorus pesticide mainly has spectral method, chromatography at present
And inhibiting AChE.Spectral method sensitivity is not high, typically can only be used for roughing as qualitatively discrimination method；Chromatography is to examine at present
Survey organophosphorus pesticide main detection method, the physicochemical characteristics in detection process can be divided into again thin-layered chromatography,
Gas chromatography and the class of high performance liquid chromatography three.Wherein gas chromatography was entered after the 1950s, in column chromatography
On the basis of a kind of new instrument analytical method for growing up, it has also become Instrumental Analysis typical, most widely used at present
Method.Thin-layered chromatography is restricted by the sensitivity analyzed, difficult quantitation.Liquid chromatography compared with gas chromatography, though
Do not limited by the volatility and heat endurance of sample, be very suitable for the analysis of macromolecular, unstable compound, but in reality
In the application of border, the sample of every energy gas chromatography analysis does not have to liquid chromatography typically, cleverer because gas-chromatography is faster
It is quick, it is more convenient, and expend lower.So gas chromatography is when analyzing organophosphorus pesticide, no matter in analyze speed, sensitivity
Or in separative efficiency, all show obvious superiority.This method is to utilize the organophosphor agriculture after extracted, purifying, concentration
Medicine injects gas chromatographic column, and after program temp rising gasifying, different organophosphorus pesticides separates in stationary phase, through different detectors
Gas chromatogram is drawn in detection scanning, by retention time come qualitative, is determined by peak height or peak area with standard curve control
Amount.Strict to use environment and operating condition requirement but gas chromatograph use condition requires high, user of service will pass through special
Training, cumbersome, the time is longer.Therefore, Quantitative detection organophosphorus pesticide can not be realized in common laboratory.
The content of the invention
It is an object of the invention to provide a kind of organophosphorus residue quantity measuring method, to solve to propose in above-mentioned background technology
The problem of.
To achieve the above object, the present invention provides following technical scheme：
A kind of organophosphorus residue quantity measuring method, is comprised the steps of,
A, sample preparation, extraction：The grain, fruit or vegetables that will likely have organophosphorus residue are dried, crushing operation, are obtained
Sample powder is obtained, sample powder is added in centrifuge tube, the polyoxyethylene list t-octyl phenyl ether aqueous solution is added, in 80-
Ultrasonic extraction l0-20min under 100kHz, and 15-20min is centrifuged under the conditions of rotating speed is 3000-3500rpm, take upper strata to extract
Liquid；
B, chromatogram gathers, and screens major influence factors using orthogonal test, several groups of preferably conditions filtered out are optimized,
Wherein sample size is 1 μ L, peak area quantified by external standard method, and the drafting of standard curve is diluted with acetone standard sample of pesticide, quality
Concentration is respectively 0.1mg/L, 0.2mg/L, 0.5mg/L, 0.8mg/L, 1.2mg/L, 2.0mg/L, every part of working solution parallel determination
5 times, be that ordinate draws standard curve using concentration as abscissa, peak area, gas flow is hydrogen 75mL/min, air
100mL/min, make-up gas 15mL/min, total carrier gas flux 60.0mL/min, 200 DEG C of injector temperature；
C, the chromatogram gathered to step B is analyzed, result of calculation.
As the further scheme of the present invention：Continuous 5 sample introductions of methods described, the relative standard deviation of retention time exist
0.01%~0.12%, the relative standard deviation of peak area is 1.8%~4.5%.
As the further scheme of the present invention：The quality of described sample powder and polyoxyethylene list t-octyl phenyl ether water
The volume ratio of solution is 1g:(28-35)mL；Polyoxy in the polyoxyethylene list t-octyl phenyl ether aqueous solution described in step 1)
The volumetric concentration of ethene list t-octyl phenyl ether is 1.5-2%.
Compared with prior art, the beneficial effects of the invention are as follows：Organophosphorus residue quantity measuring method of the present invention passes through chromatogram
The organophosphorus pesticide data that sampling analysis method is treated in detectable substance carry out quick, sensitive, accurate, easy extraction and divided
Analysis, it disclosure satisfy that farming residual analysis regulation and require.
Embodiment
The technical scheme of this patent is described in more detail with reference to embodiment.
A kind of organophosphorus residue quantity measuring method, is comprised the steps of,
A, sample preparation, extraction：The grain, fruit or vegetables that will likely have organophosphorus residue are dried, crushing operation, are obtained
Sample powder is obtained, sample powder is added in centrifuge tube, the polyoxyethylene list t-octyl phenyl ether aqueous solution is added, in 80-
Ultrasonic extraction l0-20min under 100kHz, and 15-20min is centrifuged under the conditions of rotating speed is 3000-3500rpm, take upper strata to extract
Liquid；
B, chromatogram gathers, and screens major influence factors using orthogonal test, several groups of preferably conditions filtered out are optimized,
Wherein sample size is 1 μ L, peak area quantified by external standard method, and the drafting of standard curve is diluted with acetone standard sample of pesticide, quality
Concentration is respectively 0.1mg/L, 0.2mg/L, 0.5mg/L, 0.8mg/L, 1.2mg/L, 2.0mg/L, every part of working solution parallel determination
5 times, be that ordinate draws standard curve using concentration as abscissa, peak area, gas flow is hydrogen 75mL/min, air
100mL/min, make-up gas 15mL/min, total carrier gas flux 60.0mL/min, 200 DEG C of injector temperature；
C, the chromatogram gathered to step B is analyzed, result of calculation.
Continuous 5 sample introductions of method, the relative standard deviation of retention time 0.01%~0.12%, peak area it is relative
Standard deviation is 1.8%~4.5%.Sample powder quality and the polyoxyethylene list t-octyl phenyl ether aqueous solution volume
Than for 1g:(28-35)mL；Polyoxyethylene list is tertiary pungent in the polyoxyethylene list t-octyl phenyl ether aqueous solution described in step 1)
The volumetric concentration of base phenyl ether is 1.5-2%.
The present invention operation principle be：The grain, fruit or vegetables that will likely have organophosphorus residue are dried, crushed
Operation, sample powder is obtained, sample powder is added in centrifuge tube, it is water-soluble to add polyoxyethylene list t-octyl phenyl ether
Liquid, the ultrasonic extraction lO-20min under 80-100kHz, and 15-20min is centrifuged under the conditions of rotating speed is 3000-3500rpm, take
Upper layer of extraction liquid；Major influence factors are screened using orthogonal test, several groups of preferably conditions filtered out are optimized, wherein
Sample size is 1 μ L, peak area quantified by external standard method, and the drafting of standard curve is diluted with acetone standard sample of pesticide, mass concentration
Respectively 0.1mg/L, 0.2mg/L, 0.5mg/L, 0.8mg/L, 1.2mg/L, 2.0mg/L, every part of working solution parallel determination 5
It is secondary, it is that ordinate draws standard curve using concentration as abscissa, peak area, gas flow is hydrogen 75mL/min, air
100mL/min, make-up gas 15mL/min, total carrier gas flux 60.0mL/min, 200 DEG C of injector temperature.To aforesaid operations step
The chromatogram gathered is analyzed, result of calculation.Continuous 5 sample introductions of method, the relative standard deviation of retention time is 0.01%
~0.12%, the relative standard deviation of peak area is 1.8%~4.5%.Sample powder quality and polyoxyethylene list it is tertiary pungent
The volume ratio of the base phenyl ether aqueous solution is 1g:(28-35)mL；Polyoxyethylene list t-octyl phenyl ether water described in step 1)
The volumetric concentration of polyoxyethylene list t-octyl phenyl ether is 1.5-2% in solution.
Although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of changes, modification can be carried out to these embodiments, replace without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (3)
- A kind of 1. organophosphorus residue quantity measuring method, it is characterised in that comprise the steps of,A, sample preparation, extraction：The grain, fruit or vegetables that will likely have organophosphorus residue are dried, crushing operation, are obtained Sample powder is obtained, sample powder is added in centrifuge tube, the polyoxyethylene list t-octyl phenyl ether aqueous solution is added, in 80- Ultrasonic extraction l0-20min under 100kHz, and 15-20min is centrifuged under the conditions of rotating speed is 3000-3500rpm, take upper strata to extract Liquid；B, chromatogram gathers, and screens major influence factors using orthogonal test, several groups of preferably conditions filtered out are optimized, Wherein sample size is 1 μ L, peak area quantified by external standard method, and the drafting of standard curve is diluted with acetone standard sample of pesticide, quality Concentration is respectively 0.1mg/L, 0.2mg/L, 0.5mg/L, 0.8mg/L, 1.2mg/L, 2.0mg/L, every part of working solution parallel determination 5 times, be that ordinate draws standard curve using concentration as abscissa, peak area, gas flow is hydrogen 75mL/min, air 100mL/min, make-up gas 15mL/min, total carrier gas flux 60.0mL/min, 200 DEG C of injector temperature；C, the chromatogram gathered to step B is analyzed, result of calculation.
- A kind of 2. organophosphorus residue quantity measuring method according to claim 1, it is characterised in that continuous 5 times of methods described Sample introduction, the relative standard deviation of retention time 0.01%~0.12%, the relative standard deviation of peak area 1.8%~ 4.5%。
- 3. a kind of organophosphorus residue quantity measuring method according to claim 1, it is characterised in that described sample powder Quality and the volume ratio of the polyoxyethylene list t-octyl phenyl ether aqueous solution are 1g:(28-35)mL；Polyoxy described in step 1) The volumetric concentration of polyoxyethylene list t-octyl phenyl ether is 1.5-2% in the ethene list t-octyl phenyl ether aqueous solution.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111380980A (en) * | 2020-04-21 | 2020-07-07 | 深圳市深大检测有限公司 | Method for detecting pesticide residue on fruits and vegetables |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1366065A (en) * | 2001-12-17 | 2002-08-28 | 农业部环境保护科研监测所 | Process for quickly detecting trace quantity of agricultural organophosphorus and aminoformate chemicals |
| CN1546988A (en) * | 2003-12-02 | 2004-11-17 | 厦门大学 | Rapid determination method for organophosphorus pesticide residue in vegetable and fruit |
| CN101021510A (en) * | 2007-03-02 | 2007-08-22 | 内蒙古伊利实业集团股份有限公司 | Method for checking organic phosphorus pesticide residue in animal milk |
| CN104597173A (en) * | 2013-10-31 | 2015-05-06 | 大连大公环境检测有限公司 | Organophosphorus pesticide residue determination method |
| 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 |
-
2017
- 2017-10-27 CN CN201711018326.7A patent/CN107831257A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1366065A (en) * | 2001-12-17 | 2002-08-28 | 农业部环境保护科研监测所 | Process for quickly detecting trace quantity of agricultural organophosphorus and aminoformate chemicals |
| CN1546988A (en) * | 2003-12-02 | 2004-11-17 | 厦门大学 | Rapid determination method for organophosphorus pesticide residue in vegetable and fruit |
| CN101021510A (en) * | 2007-03-02 | 2007-08-22 | 内蒙古伊利实业集团股份有限公司 | Method for checking organic phosphorus pesticide residue in animal milk |
| CN104597173A (en) * | 2013-10-31 | 2015-05-06 | 大连大公环境检测有限公司 | Organophosphorus pesticide residue determination method |
| 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 |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111380980A (en) * | 2020-04-21 | 2020-07-07 | 深圳市深大检测有限公司 | Method for detecting pesticide residue on fruits and vegetables |
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Application publication date: 20180323 |