CN106596776B - The pre-treating method of pyrethroid pesticide remained test sample in grape wine - Google Patents
The pre-treating method of pyrethroid pesticide remained test sample in grape wine Download PDFInfo
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- CN106596776B CN106596776B CN201611182093.XA CN201611182093A CN106596776B CN 106596776 B CN106596776 B CN 106596776B CN 201611182093 A CN201611182093 A CN 201611182093A CN 106596776 B CN106596776 B CN 106596776B
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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
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Abstract
The invention discloses a kind of pre-treating methods of pyrethroid pesticide remained test sample in grape wine, the present invention is extractant using the ethyl alcohol contained in grape wine, enough dehydrating agents (anhydrous magnesium sulfate, anhydrous sodium sulfate), split-phase salt (ammonium sulfate, dipotassium hydrogen phosphate), cleanser (N- propyl ethylenediamine) are once added directly in grape wine, centrifuging and taking supernatant directly carries out chromatography, mass spectral analysis.It is simple and reliable that aspect of the invention realizes the residual extraction of agriculture, concentration and purification, method in single stepping.
Description
Technical field
The present invention relates to Detecting Pesticide fields, more particularly to pyrethroid pesticide remained in a kind of grape wine
The pre-treating method of test sample.
Background technique
Pyrethroid is common broad spectrum insecticide, and the residual of such pesticide can cause human body in bag and bottle
Injury.Some researches show that pyrethroids can upset the normal physiological of animal nerve, and then generates harm to animal.At present
There are many countries to have done strict control to the residual quantity of pyrethroid in food, beverage.For agricultures such as melon fruits and vegetables, cereals
The detection of pyrethroid has more report in the processing agricultural product such as crop and vegetable oil, grape wine.
Pyrethroid pesticide remained method for quantitatively determining is mainly gas chromatography, gas phase color in existing grape wine
Spectrum-Mass Spectrometry.These measuring methods are sensitive, accurate, accurate, but need to sample carry out pre-treatment (extract, concentration,
Purification).
Currently, the standard pre-treating method of Pesticide Residues in Wine measurement is solvent extraction combination Solid Phase Extraction column purification
Concentration, this method operating procedure is tediously long, and needs to consume a large amount of organic solvents, and extraction efficiency is relatively low.Therefore, it studies in grape wine
The quick detection pre-treating method of pyrethroid pesticide remained measurement is very necessary.
QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method earliest by
Anastassiades, M. propose that it uses acetonitrile for extract liquor, and anhydrous MgSO is added in extract liquor4Water removal, and chlorine is added
Change sodium as split-phase salt, then takes supernatant that direct injection analysis after cleanser (N- propyl ethylenediamine etc.) purification is added.
QuEChERS method is used widely in the samples such as veterinary antibiotics.Currently, there is researcher to be introduced into QuEChERS method
In the sample pre-treatments of grape wine detection, preferable effect is achieved.However, there is still a need for extract liquor second is added for QuEChERS method
Nitrile, extracting solution is not by concentration, and there is still a need for further purify to extracting solution.
Summary of the invention
The object of the present invention is to provide a kind of pre-treatment sides of pyrethroid pesticide remained test sample in grape wine
Method, the one-step method Sample Pretreatment Technique of pyrethroid pesticide remained detection in especially a kind of grape wine, i.e., in a step
It realizes that agriculture is residual in operation to extract, be concentrated and purify.
It is a further object of the present invention to provide a kind of methods of pyrethroid pesticide remained detection in grape wine.
The pre-treating method of pyrethroid pesticide remained test sample in grape wine, comprising the following steps: take certain
The grape wine of amount is added at one time enough dehydrating agents, split-phase salt and cleanser, vibrates, and centrifugation takes supernatant directly to carry out reality
Test is fixed.
The pre-treating method of pyrethroid pesticide remained test sample in grape wine of the present invention, wherein institute
The dehydrating agent stated is at least one of anhydrous magnesium sulfate or anhydrous sodium sulfate；The split-phase salt is sodium chloride, ammonium sulfate, phosphoric acid
At least one of hydrogen dipotassium；The cleanser is N- propyl ethylenediamine；
The dosage of the grape wine is denoted as X mL, and the dosage of dehydrating agent is then 0.2X~0.4X g；The dosage of split-phase salt is then
For 0.2X~0.4X g；The dosage of cleanser is then 10X~30X mg.
The pre-treating method of pyrethroid pesticide remained test sample in grape wine of the present invention, wherein tool
Body is shaken up, accurately measures 10.00mL, be placed in 20mL plastic centrifuge tube the following steps are included: take 1 bottle of grape wine, it is disposable plus
Enter enough dehydrating agents, split-phase salt and cleanser, vortex oscillation 2min, in 4000rmin-1Lower centrifugation, then directly takes upper layer
Clear liquid carries out measuring.
The pre-treating method of pyrethroid pesticide remained test sample in grape wine of the present invention, wherein institute
The dosage for stating dehydrating agent is 2-4g；The dosage of the split-phase salt is 2-4g；The dosage of the cleanser is 100-300mg.
The pre-treating method of pyrethroid pesticide remained test sample in grape wine of the present invention, wherein institute
Stating ethanol content in grape wine is 12%-13%.
The pre-treating method of pyrethroid pesticide remained test sample carries out grape in grape wine of the present invention
The method of pyrethroid pesticide remained detection in wine, specifically includes the following steps:
(1) 1 bottle of grape wine without pesticide residue is taken, alcohol content is denoted as A%, it shakes up,
(2) 10.00mL is accurately measured, is placed in 20mL plastic centrifuge tube, enough dehydrating agents, split-phase salt are added at one time
And cleanser, vortex oscillation 2min, in 4000rmin-1Lower centrifugation, directly takes supernatant liquor to be measured, this measurement result is
Blank sample；
(3) 3 parts of grape wine of 10.00mL are accurately measured, 10 μ L of pestsides synthesis standard solution is separately added into, is added at one time
With the dehydrating agent, split-phase salt and cleanser of step 2 moderate, vortex oscillation 2min, in 4000rmin-1Lower centrifugation, directly takes
Supernatant liquor carries out determination of recovery rates, and calibration curve method calculates measurement result.
The method of pyrethroid pesticide remained detection in grape wine of the present invention, wherein the pestsides synthesis
Standard solution be 6 kinds of pestsides synthesis form, including tetramethrin, Fenpropathrin, lambda-cyhalothrin, cypermethrin, fenvalerate and
Decis, concentration are 10 μ g/mL.
The method of pyrethroid pesticide remained detection in grape wine of the present invention, wherein determination of recovery rates item
Part and method are as follows:
GC-ECD condition, DB-1701 quartz capillary chromatographic column, 30.0m × 0.25mm × 0.25 μm, Japanese Shimadzu are public
Department, stationary phase are methyl polysiloxane coating, weak/middle polarity；
Chromatogram column temperature is set by temperature programming: 220 DEG C of initial temperature, 1min is kept, with 5 DEG C of min-1It is warming up to 250
DEG C, then with 20 DEG C of min-1280 DEG C are warming up to, 15min is kept；Injector temperature is 280 DEG C；Detector is 300 DEG C；Sample introduction
Amount is 1 μ L, split sampling, split ratio 20；
Quantitative approach is standard curve standard measure, if measurement result is X, pesticide concentration C=X/ (100/ in wine samples
A) μ g/mL, A are alcohol content.
The method of the present invention compared with prior art, protrudes effect and is:
(1) the method for the present invention is a kind of sample-pretreating method quickly, accurate, easy.Contain 12%- in grape wine
Appropriate dehydrating agent (anhydrous magnesium sulfate, anhydrous sodium sulfate), split-phase salt (sodium chloride, ammonium sulfate, phosphoric acid hydrogen is added in 13% ethyl alcohol
Dipotassium) when, water and water colo(u)r, tannin under salting out in ethyl alcohol and grape wine are layered, fat-soluble pesticide residue into
Enter upper layer, since the content of ethyl alcohol is less, exactly plays the effect of extracting solution concentration, meanwhile, N- is added in extraction process
Propyl ethylenediamine can effectively adsorpting pigment, play catharsis.
(2) the method for the present invention can be to six kinds of common pyrethroid drug (tetramethrin, Fenpropathrin, lambda-cyhalothrin, chlorine
Cyano chrysanthemate, fenvalerate and decis) realize rapid and accurate determination.
(3) the method for the present invention is environmentally protective, and detection limit is low, accuracy is high, precision is good.
Explanation and specific embodiment are residual to pyrethroid pesticide in grape wine of the present invention with reference to the accompanying drawing
The pre-treating method of test sample is stayed to be described further.
Detailed description of the invention
Fig. 1 is the chromatogram that pestsides synthesis standard solution is added in organic claret.
Specific embodiment
Embodiment 1 is using the pre-treating method of pyrethroid pesticide remained test sample in grape wine to organic extra dry red wine
The detection of wine samples recovery of standard addition is tested
1 bottle of organic claret without pesticide residue is taken, alcohol content 12.5% shakes up, accurate to measure
10.00mL is placed in 20mL plastic centrifuge tube, and disodium hydrogen phosphate 2g, anhydrous magnesium sulfate 3g, N- propyl ethylenediamine 150mg is added,
Vortex oscillation 2min is centrifuged (4000rmin-1), then, directly supernatant liquor is taken to be measured, this measurement result is blank sample
Product.
Aforesaid operations are same as, 3 portions of organic clarets of 10.00mL are taken, are separately added into 10 μ L of pestsides synthesis standard solution,
Determination of recovery rates is carried out, calibration curve method calculates measurement result.The pestsides synthesis standard solution is that 6 kinds of pestsides synthesis form,
Including tetramethrin, Fenpropathrin, lambda-cyhalothrin, cypermethrin, fenvalerate and decis, concentration is 10 μ gmL-1。
Chromatogram after sample addition pesticide standard is as shown in Figure 1.Wherein, tetramethrin (9.992), Fenpropathrin
(9.931), lambda-cyhalothrin (11.581), cypermethrin (12.19), fenvalerate (14.211) and decis
(15.153), concentration is added is 10 μ gmL-1。
Wherein, determination of recovery rates condition and method are as follows:
GC-ECD condition, (30.0m × 0.25mm × 0.25 μm, Japanese Shimadzu are public for DB-1701 quartz capillary chromatographic column
Department, stationary phase are methyl polysiloxane coating, weak/middle polarity)；
Chromatogram column temperature is set by temperature programming: 220 DEG C of initial temperature, 1min is kept, with 5 DEG C of min-1It is warming up to 250
DEG C, then with 20 DEG C of min-1280 DEG C are warming up to, 15min is kept；Injector temperature is 280 DEG C；Detector is 300 DEG C；Sample introduction
Amount is 1 μ L, split sampling, split ratio 20.
Quantitative approach is standard curve standard measure, if measurement result is X, pesticide concentration C (μ g/mL) in wine samples
Are as follows: C=X/ (100/12.5), 12.5 be alcohol content V/V, if alcohol content variation formula is analogized.
The organic claret recovery testu measurement result (n=3) of table 1
Measurement result shows: the pre-treating method of pyrethroid pesticide remained test sample is applied to have in grape wine
In machine red wine measure pyrethroid pesticide the rate of recovery between 81.1-93.1%, RSD 0.658-5.41% it
Between.Detection limit is lower than 0.003 μ g/mL.
The pre-treating method of pyrethroid pesticide remained test sample is to claret sample in 2 grape wine of embodiment
The detection of product is tested
Take 1 bottle of claret, alcohol content 12.0% shakes up, accurately measures 10.00mL, be placed in 20mL plastics from
In heart pipe, ammonium sulfate 3g, anhydrous sodium sulfate 2g, N- propyl ethylenediamine 200mg, vortex oscillation 2min is added, is centrifuged (4000r
min-1), then, directly supernatant liquor is taken to be measured, this measurement result is blank sample.
Aforesaid operations are same as, 3 portions of 10.00mL clarets are taken, are separately added into 10 μ L of pestsides synthesis standard solution, are carried out
Determination of recovery rates, calibration curve method calculate measurement result.The pestsides synthesis standard solution forms for 6 kinds of pestsides synthesis, including
Tetramethrin, Fenpropathrin, lambda-cyhalothrin, cypermethrin, fenvalerate and decis, concentration are 10 μ gmL-1。
Determination of recovery rates condition and method are same as Example 1.
The result shows that: it is not detected in claret pyrethroid pesticide remained.Pesticide standard solution is added in sample
Chromatogram afterwards is substantially the same manner as Example 1.Recovery of standard addition is 82-96%.
The pre-treating method of pyrethroid pesticide remained test sample is to dry white wine sample in 3 grape wine of embodiment
The detection of product is tested
Take 1 bottle of dry white wine, alcohol content 12.0% shakes up, accurately measures 10.00mL, be placed in 20mL plastics from
In heart pipe, dipotassium hydrogen phosphate 3g, 4 grams of anhydrous sodium sulfate, N- propyl ethylenediamine 100mg, vortex oscillation 2min, centrifugation is added
(4000r·min-1), then, directly supernatant liquor is taken to be measured, this measurement result is blank sample.
Aforesaid operations are same as, 3 portions of 10.00mL dry white wines are taken, are separately added into 10 μ L of pestsides synthesis standard solution, are carried out
Determination of recovery rates, calibration curve method calculate measurement result.The pestsides synthesis standard solution forms for 6 kinds of pestsides synthesis, including
Tetramethrin, Fenpropathrin, lambda-cyhalothrin, cypermethrin, fenvalerate and decis, concentration are 10 μ gmL-1。
Determination of recovery rates condition and method are same as Example 1.
The result shows that: it is not detected in dry white wine pyrethroid pesticide remained.Pesticide standard solution is added in sample
Chromatogram and embodiment 1 afterwards, it is essentially identical.Recovery of standard addition is 84.5-95.0%.
The pre-treating method of pyrethroid pesticide remained test sample is to ice red wine sample in 4 grape wine of embodiment
The detection of product is tested
1 bottle of dry ice red wine is taken, alcohol content 13.0% shakes up, accurately measures 10.00mL, is placed in 20mL plastics
In centrifuge tube, ammonium sulfate 4g, 2 grams of anhydrous magnesium sulfate, N- propyl ethylenediamine 300mg, vortex oscillation 2min, centrifugation is added
(4000r·min-1), then, directly supernatant liquor is taken to be measured, this measurement result is blank sample.
Aforesaid operations are same as, 3 portions of 10.00mL ice red wine are taken, are separately added into 10 μ L of pestsides synthesis standard solution, are carried out
Determination of recovery rates, calibration curve method calculate measurement result.The pestsides synthesis standard solution forms for 6 kinds of pestsides synthesis, including
Tetramethrin, Fenpropathrin, lambda-cyhalothrin, cypermethrin, fenvalerate and decis, concentration are 10 μ gmL-1。
Determination of recovery rates condition and method are same as Example 1.
The result shows that: it is not detected in ice red wine pyrethroid pesticide remained.Pesticide standard solution is added in sample
Chromatogram and embodiment 1 afterwards, it is essentially identical.Recovery of standard addition is 84.1-98.2%.
Embodiment described above only describe the preferred embodiments of the invention, not to model of the invention
It encloses and is defined, without departing from the spirit of the design of the present invention, those of ordinary skill in the art are to technical side of the invention
The various changes and improvements that case is made should all be fallen into the protection scope that claims of the present invention determines.
Claims (8)
1. the pre-treating method of pyrethroid pesticide remained test sample in a kind of grape wine, it is characterised in that: including with
Lower step: taking a certain amount of grape wine, is added at one time enough dehydrating agents, split-phase salt and cleanser, vibrates, and centrifugation takes
Clear liquid directly carries out measuring；The cleanser is N- propyl ethylenediamine.
2. the pre-treating method of pyrethroid pesticide remained test sample in grape wine according to claim 1,
Be characterized in that: the dehydrating agent is at least one of anhydrous magnesium sulfate or anhydrous sodium sulfate；The split-phase salt be sodium chloride,
At least one of ammonium sulfate, dipotassium hydrogen phosphate；
The dosage of the grape wine is denoted as X mL, and the dosage of dehydrating agent is then 0.2X~0.4X g；The dosage of split-phase salt is then
0.2X~0.4X g；The dosage of cleanser is then 10X~30X mg.
3. the pre-treating method of pyrethroid pesticide remained test sample in grape wine according to claim 2,
It is characterized in that: specifically includes the following steps: taking 1 bottle of grape wine, shaking up, accurately measure 10.00mL, be placed in 20mL plastic centrifuge tube
In, it is added at one time enough dehydrating agents, split-phase salt and cleanser, vortex oscillation 2min, in 4000rmin-1Lower centrifugation, so
Supernatant liquor is directly taken to carry out measuring afterwards.
4. the pre-treating method of pyrethroid pesticide remained test sample in grape wine according to claim 3,
Be characterized in that: the dosage of the dehydrating agent is 2-4g；The dosage of the split-phase salt is 2-4g；The dosage of the cleanser is 100-
300mg。
5. the pre-treating method of pyrethroid pesticide remained test sample in grape wine according to claim 4,
Be characterized in that: ethanol content is 12%-13% in the grape wine.
6. using the preceding place of pyrethroid pesticide remained test sample in grape wine of any of claims 1-5
The method that reason method carries out pyrethroid pesticide remained detection in grape wine, it is characterized in that: the following steps are included:
(1) 1 bottle of grape wine without pesticide residue is taken, alcohol content is denoted as A%, it shakes up,
(2) 10.00mL is accurately measured, is placed in 20mL plastic centrifuge tube, enough dehydrating agents, split-phase salt and net are added at one time
Agent, vortex oscillation 2min, in 4000rmin-1Lower centrifugation, directly takes supernatant liquor to be measured, this measurement result is blank
Sample；
(3) 3 parts of grape wine of 10.00mL are accurately measured, 10 μ L of pestsides synthesis standard solution is separately added into, is added at one time and walks
Dehydrating agent, split-phase salt and the cleanser of rapid 2 moderate, vortex oscillation 2min, in 4000rmin-1Lower centrifugation, directly takes upper layer
Clear liquid carries out determination of recovery rates, and calibration curve method calculates measurement result.
7. pyrethroid pesticide remained detection method in grape wine according to claim 6, it is characterised in that: described
Pestsides synthesis standard solution forms for 6 kinds of pestsides synthesis, including tetramethrin, Fenpropathrin, lambda-cyhalothrin, cypermethrin, cyanogen
Valerate and decis, concentration are 10 μ g/mL.
8. pyrethroid pesticide remained detection method in grape wine according to claim 7, it is characterised in that: recycling
Rate determination condition and method are as follows:
GC-ECD condition, DB-1701 quartz capillary chromatographic column, 30.0m × 0.25mm × 0.25 μm, Japanese Shimadzu Corporation, Gu
Fixed is mutually methyl polysiloxane coating, weak/middle polarity；
Chromatogram column temperature is set by temperature programming: 220 DEG C of initial temperature, 1min is kept, with 5 DEG C of min-1250 DEG C are warming up to, after
And with 20 DEG C of min-1280 DEG C are warming up to, 15min is kept；Injector temperature is 280 DEG C；Detector is 300 DEG C；Sample volume is 1
μ L, split sampling, split ratio 20；
Quantitative approach is standard curve standard measure, if measurement result is X, pesticide concentration C=X/ (100/A) μ in wine samples
G/mL, A are alcohol content.
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| CN110346344A (en) * | 2018-11-14 | 2019-10-18 | 厦门市普识纳米科技有限公司 | A kind of detection method of pesticide residue containing Cyano chrysanthemate |
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