CN107121511A - A kind of method of high flux quick detection edible mushroom Pesticide Residues - Google Patents
A kind of method of high flux quick detection edible mushroom Pesticide Residues Download PDFInfo
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- CN107121511A CN107121511A CN201710324577.1A CN201710324577A CN107121511A CN 107121511 A CN107121511 A CN 107121511A CN 201710324577 A CN201710324577 A CN 201710324577A CN 107121511 A CN107121511 A CN 107121511A
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Abstract
The present invention relates to a kind of method of high flux quick detection edible mushroom Pesticide Residues, belong to Agricultural Food Analysis detection technique field.This method is based on gas chromatography combined with mass spectrometry technology（GC‑MS）, by setting up triple Database Systems, quick detection and the examination of edible mushroom Pesticide Residues are realized, step includes：Full-automatic sample pretreatment, GC MS are determined and triple database screening system is quickly analyzed.The present invention can realize the content for assessing edible mushroom Pesticide Residues, realize high flux, full automatic residues of pesticides Screening analysis according to different instance model calibration curve databases.
Description
Technical field
The present invention relates to a kind of method of quick detection edible mushroom Pesticide Residues, belong to Agricultural Food Analysis detection technique neck
Domain.
Background technology
China is Edible Fungi maximum in the world, big export country, with edible fungus industrial cultivation technology gradually
Maturation, mushroom industry is gradually developed, and particularly asparagus, the cultivation amount of pleurotus eryngii increase year by year, edible mushroom production,
Safety problem in sale, process is also increasingly paid attention to.Edible mushroom is in plantation, harvesting, transport and sales process
The poisonous and harmful substances such as residues of pesticides, environmental contaminants, container package additive, formaldehyde, sulfur dioxide, poisonous metal are asked safely
Topic is increasingly subject to attention both at home and abroad.But China's food safety risk supervision work still suffers from monitoring capability deficiency, specified risk material
The problems such as examination is difficult, mechanism detectability difference in each department is big, still there is larger gap with developed country, solves edible mushroom safety
Problem turns into the urgent task of China's Edible Fungi Industry Development, and the production of edible mushroom also will will be from pursuit scalar type to quality
Profit evaluation model direction changes.
The analysis of Pesticide Residues is main to be made up of the extraction and cleaning pre-treatment and detection two parts of sample, at present,
Conventional preconditioning technique mainly has SPE（SPE）, supercritical fluid extraction（SFE）, microwave auxiliary extraction（MAE）, base
Matter solid phase dispersion is extracted（MSPDE）Deng, these traditional Pesticide Residues preprocess method often sample requirements it is big,
Extract and purifying step complexity is cumbersome, operating time length, solvent consumption are big so that the detection efficiency of Residual Pesticides in Farm Produce is big
Big to decline, the safety monitoring for often leading to many agricultural product is seriously delayed.In terms of detection technique, method has a lot, mainly has
Inhibiting AChE, ELISA, light splitting brightness method, chromatography and mass spectrography etc., these assay methods are qualitative fixed in raising agricultural chemicals
Huge effect is played in terms of amount quick detection, but often has that sample requirements are big, need preparing standard solution etc. to ask
Topic.
At present, domestic researcher is typically to be built to scheme with standard items in the research to food risk compound examination
Spectrum storehouse comes qualitative to object and quantitative, or utilizes existing spectrum storehouse（NIST）It is qualitative then with standard items make standard curve
To quantify.Some researchs also establish several carbamates and organo-chlorine pesticide in the edible mushrooms such as mushroom, pleurotus eryngii, White mushroom
The GC-MS assay methods of residual.But existing analysis method is carried out just for a specific several or class specific objective thing
Detection, and for being likely to be present in food but not being that target class material this type organic can not then carry out examination, it is difficult to realize
Full scan and examination are carried out to all residues of pesticides.Need to prepare its standard liquid and make when residues of pesticides are quantitatively detected to mark
Directrix curve, analysis throughput is relatively low, it is also difficult to realize being analyzed together with the multicomponent under identical conditions for unification.
The content of the invention
It is an object of the present invention in view of the above-mentioned problems, provide a kind of high flux quick detection edible mushroom Pesticide Residues
Method, step is：
（1）Full-automatic Sample Pretreatment Technique Used：Extract：Every gram of edible mushroom sample adds 2 mL acetonitriles, and 2 min are extracted in homogenate, plus
Enter and centrifuged after 0.4 g anhydrous magnesium sulfates and 0.1 g sodium chloride, the min of vortex oscillation 1, take supernatant concentrated by rotary evaporation to be done near, plus
1mL acetonitriles dissolve, and cross 0.22 μm of filter membrane to be determined.
Extraction：Extracted using the stirring rod for scribbling poly- dimethoxysiloxane.Stirring rod is heated at 300 DEG C
40min, nitrogen flow rate 1.2mL/min, 1000r/min stirs 45min during extraction.
（2）GC-MS is determined：Chromatographic condition：Chromatogram column temperature program：70 DEG C of initial temperature, keeps 2min, with 25 DEG C/min
150 DEG C are risen to, 200 DEG C are risen to 3 DEG C/min, 280 DEG C are risen to 8 DEG C/min, 10min is kept；Carrier gas：High-purity helium, purity
≥99.999%；Flow rate of carrier gas 1.0mL/min；Injector temperature：280℃；Solvent delay：3.5min；Input mode：Do not shunt
Sample introduction；Sample size：2µl.
Mass Spectrometry Conditions：Ionization mode：EI；Electron energy 70eV；230 DEG C of ion source temperature；150 DEG C of level Four bar temperature；Matter
Compose tuning manner：DFTPP is tuned, and resolution ratio and sensitivity reach best match.Scan mode：Full scan pattern, scans matter
Measure scope 35~550, sweep speed：2.86scan/sec.
（3）Triple Database Systems based on GC-MS：By retention time database, MS spectrum spectrum library, compound school
Demonstrate,prove curve composition.
The method of quick detection edible bacterium residues of pesticides of the present invention, utilizes full-automatic pretreatment and GC-MS combination ternarys
The quick screening method of group Database edible mushroom Determination of Multiple Pesticide Residues, the rapid screening for edible mushroom sample is provided reliably
Technical support and more fast and convenient solution route, present invention can apply to the quick disposal of edible mushroom sample accident
Emergency, greatly shortens the analysis time of sample, improves the operating efficiency of detection examination.
Full-automatic sample pretreatment solves that edible mushroom Pesticide Residues sample requirements in preprocessing process are big, extract and
Purifying step complexity is cumbersome, operating time length, the problems such as solvent consumption is big, cost is high, human error is disturbed, method flexibly, it is high
Flux and energy rapid screening.Dynamic Headspace effectively reduces the usage amount of organic solvent, is also kept away using high-purity gas extraction
Exempt from solvent and introduce disturbing factor.The quick screening method of GC-MS technology combination triple Databases need not prepare mark
Quasi- solution and making standard curve, it is not necessary to the harmful substance that standard substance comes in qualitative/quantitative sample, directly pass through and calibrate bent
Line database can just assess the content of medicine and agricultural chemicals, short, Ke Yijian the time required to automatic detection and quantitative chemical risk thing
Residues of pesticides are surveyed, environmental contaminants, nearly 100 kinds of compounds of the multicomponent analysis of container package additive etc. are effectively solved
The screening of edible mushroom risk thing is difficult, detection speed is slow, it is big to obtain data difference, and needs in traditional analysis preparation standard
Solution carries out the problems such as manpower, financial resources, material resources spent during qualitative/quantitative analysis.
Embodiment
The method and feature of the present invention are described below in conjunction with instantiation, example is served only for explaining this hair
It is bright, it is not intended to limit the scope of the present invention.
Residues of pesticides in embodiment detection mushroom
Precise 10.0000g mushrooms sample adds 20mL acetonitriles, and 2min is extracted in homogenate, adds 4g anhydrous magnesium sulfates and 1g chlorine
Change sodium, vortex oscillation 1min, 4000r/min centrifugation 10min takes supernatant concentrated by rotary evaporation to be done near, plus the dissolving of 1mL acetonitriles, mistake
0.22 μm of filter membrane is to be determined.
Extracted using the stirring rod for scribbling poly- dimethoxysiloxane, set stirring rod to be heated at 300 DEG C
40min, nitrogen flow rate 1.2mL/min, 1000r/min stirs 45min during extraction.
GC-MS is determined：Chromatographic condition：Chromatogram column temperature program：70 DEG C of initial temperature, keeps 2min, with 25 DEG C/min liters
To 150 DEG C, 200 DEG C are risen to 3 DEG C/min, 280 DEG C are risen to 8 DEG C/min, 10min is kept；Carrier gas：High-purity helium, purity >=
99.999%；Flow rate of carrier gas 1.0mL/min；Injector temperature：280℃；Solvent delay：3.5min；Input mode：It is not diverted into
Sample；Sample size：2µl.
Mass Spectrometry Conditions：Ionization mode：EI；Electron energy 70eV；230 DEG C of ion source temperature；150 DEG C of level Four bar temperature；Matter
Compose tuning manner：DFTPP is tuned, and resolution ratio and sensitivity reach best match.Scan mode：Full scan pattern, scans matter
Measure scope 35~550, sweep speed：2.86scan/sec.
Triple Database Systems based on GC-MS are set up, spectrum library, compound are composed by retention time database, MS
The retention time of common agricultural chemicals in school card curve composition, the 18 kinds of edible mushrooms thus improved and set up, object ion and quantitative
Ion database.Triple database detects compound automatically and relative quantification is only needed 2 minutes.Detection is limited to 0.001 mg/kg
~0.050 mg/kg, average recovery rate is 79%~110%, and relative standard deviation is 1.0%~5.8%, complies fully with residues of pesticides
The requirement of analysis method.Result of the test shows that this method is simple to operate, sensitivity is high, favorable reproducibility, can meet edible mushroom middle peasant
The examination detection of medicine residual is required.
Claims (2)
1. a kind of method of high flux quick detection edible mushroom Pesticide Residues, it is characterised in that：Three below step is connected
Get up：
（1）Full-automatic sample pretreatment；
（2）GC-MS is determined；
（3）Quickly analysis and the examination of triple database.
2. a kind of method of high flux quick detection edible mushroom Pesticide Residues according to claim 1, it is characterised in that：
Comprise the following steps that：
（1）Full-automatic sample pretreatment：Extract：Every gram of edible mushroom sample adds 2mL acetonitriles, and homogenate is extracted, and adds 0.4 g anhydrous
Centrifuged after magnesium sulfate and 0.1 g sodium chloride, vortex oscillation, take supernatant rotary evaporation to be done near, plus the dissolving of 1mL acetonitriles, mistake
0.22 μm of filter membrane is to be determined；
Extraction：Extracted using the stirring rod for scribbling poly- dimethoxysiloxane, stirring rod heats 40min, nitrogen at 300 DEG C
Gas velocity 1.2mL/min, 1000r/min stirs 45min during extraction；
（2）GC-MS is determined：Chromatographic condition：Chromatogram column temperature program：70 DEG C of initial temperature, is kept 2min, is risen to 25 DEG C/min
150 DEG C, 200 DEG C are risen to 3 DEG C/min, 280 DEG C are risen to 8 DEG C/min, 10min is kept；Carrier gas：High-purity helium, purity >=
99.999%；Flow rate of carrier gas 1.0mL/min；Injector temperature：280℃；Solvent delay：3.5min；Input mode：It is not diverted into
Sample；Sample size：2µl；
Mass Spectrometry Conditions：Ionization mode：EI；Electron energy 70eV；230 DEG C of ion source temperature；150 DEG C of level Four bar temperature；Mass spectrum is adjusted
Humorous mode：DFTPP is tuned, and resolution ratio and sensitivity reach best match；Scan mode：Full scan pattern, quality of scanning model
Enclose 35~550, sweep speed：2.86scan/sec；
（3）Triple Database Systems based on GC-MS：Demonstrate,prove bent by the school of retention time database, MS spectrums spectrum library, compound
Line is constituted.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109187871A (en) * | 2018-09-20 | 2019-01-11 | 东莞市北扬工业设计有限公司 | A kind of test device for indoor formaldehyde |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN105717232A (en) * | 2016-02-23 | 2016-06-29 | 中华人民共和国济宁出入境检验检疫局 | Method for detecting residual organo-chlorine pesticide through stir bar sorptive extraction |
| CN105738514A (en) * | 2016-02-23 | 2016-07-06 | 中华人民共和国济宁出入境检验检疫局 | Method for detecting pesticide residues through stirring rod adsorption and extraction |
-
2017
- 2017-05-10 CN CN201710324577.1A patent/CN107121511A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN105717232A (en) * | 2016-02-23 | 2016-06-29 | 中华人民共和国济宁出入境检验检疫局 | Method for detecting residual organo-chlorine pesticide through stir bar sorptive extraction |
| CN105738514A (en) * | 2016-02-23 | 2016-07-06 | 中华人民共和国济宁出入境检验检疫局 | Method for detecting pesticide residues through stirring rod adsorption and extraction |
Non-Patent Citations (2)
| Title |
|---|
| 曾凡刚: "SBSE-TDU-GC快速测定茶叶中7种拟除虫菊酯类农药残留", 《农药》 * |
| 胡秋辉等: "固相萃取-气相色谱-质谱联用法筛查食用菌中的农药残留", 《食品科学》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109187871A (en) * | 2018-09-20 | 2019-01-11 | 东莞市北扬工业设计有限公司 | A kind of test device for indoor formaldehyde |
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