CN108226343A - Multiple Pesticides method for detecting residue in a kind of vegetables and fruits - Google Patents
Multiple Pesticides method for detecting residue in a kind of vegetables and fruits Download PDFInfo
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- CN108226343A CN108226343A CN201810016674.9A CN201810016674A CN108226343A CN 108226343 A CN108226343 A CN 108226343A CN 201810016674 A CN201810016674 A CN 201810016674A CN 108226343 A CN108226343 A CN 108226343A
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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 embodiment of the invention discloses Multiple Pesticides method for detecting residue in a kind of vegetables and fruits, including：Extracting solution is added in vegetables and fruits sample to be uniformly mixed, and sodium chloride is added in after mechanical shaking extraction, again after mixing, centrifuging treatment obtains stratified liquid；It purifies and anhydrous magnesium sulfate, PSA and C18 fillers is added in pipe；The supernatant liquor of gained liquid is pipetted to purification pipe mesoscale eddies and is mixed, is centrifuged score layer liquid after processing；The supernatant liquor of gained liquid is pipetted respectively to two reception pipes, drying obtains extract, and first reception pipe adds in n-hexane, and second reception pipe adds in first alcohol and water；The solution in first reception pipe is filtered, filtered fluid is detected using gas-chromatography tandem mass spectrometry；The solution in second reception pipe is filtered, filtered fluid is detected using liquid chromatography tandem mass spectrometry.The embodiment of the present invention reduces the time spent in purification process, so as to improve the residual detection efficiency of vegetables and fruits agriculture.
Description
Technical field
The present invention relates to gas/liquid phase chromatography-tandem mass spectrum detection technique field, Multiple Pesticides in more particularly to a kind of vegetables and fruits
Method for detecting residue.
Background technology
Pesticide is protecting crops not receive disease pest and weed harm, is improving agricultural production as important capital goods in the agricultural sector
Efficiency ensures that crop yield etc. plays a crucial role, but simultaneously because the unreasonable use of pesticide, leads to agriculture
Medicine residual is exceeded, also damages to public's health and food security.With being constantly progressive for pesticide industry, use at present
Pesticide variety and quantity also constantly increasing.The safety issue of agricultural product is always the focus of social concerns, direct relation
To public health and ecological environment security.At present, pesticide residue analysis method is to evaluate the weight of agricultural product quality and safety level
Want one of means.Wherein, gas (liquid) phase chromatography-tandem mass spectrum technology is since it is with high sensitivity, selective strong, qualitative tool
The advantages such as reliable and analysis time is short and the favor for receiving pesticide residue researcher, the technology are widely used in complex matrices background
Under trace materials detection.
Vegetable and fruit is one of most important edible agricultural product in the world, with the raising of Chinese society economic level, vegetable
Ratio of the dish fruit in public's diet is continuously improved.Meanwhile most vegetables fruit is short, sick away from harvesting interval with listing
Insect pest is commonplace, the costly feature of crop economy, causes applying pesticides type and dosage in production relatively more, therefore vegetable
Dish pesticide residues in fruits excessive problem protrudes.
Pesticides Testing method in existing vegetable and fruit, generally use gas chromatography-mass spectrography and liquid chromatography-tandem matter
Spectrometry generally comprises fruit tree middle peasant residual extraction, the purification of extracting solution.The prior art usually requires to pass through Solid Phase Extraction
Column purification extracting solution, the characteristics of due to solid-phase extraction column itself, in purification process, operating procedure is complicated, the control of method key
Point is more, and purification is caused to spend more time, reduces whole detection efficiency.
Invention content
The embodiment of the invention discloses Multiple Pesticides method for detecting residue in a kind of vegetables and fruits, are detected in vegetable and fruit with improving
The detection efficiency of pesticide residue.Technical solution is as follows：
Multiple Pesticides method for detecting residue in a kind of vegetables and fruits, including：
A) extracting solution is added in vegetables and fruits sample, after mixing, 5~30min of mechanical shaking extraction adds sodium chloride, then
It is secondary to be centrifuged handling after mixing, obtain the liquid of lower leaf；
B) anhydrous magnesium sulfate, PSA and C18 fillers are added in pipe is purified, wherein, between anhydrous magnesium sulfate, PSA and C18
Volume ratio is 4：1~3：3~1, obtain the purification pipe equipped with filler；
C) supernatant liquor of liquid obtained by step a) is pipetted into the purification pipe equipped with filler, 1~2min of vortex mixed,
After being centrifuged processing, stratified liquid up and down is obtained；
D) supernatant liquor in the stratified liquid up and down for obtaining step c) is pipetted respectively into two reception pipes, and respectively
Drying, obtains extract, n-hexane is added in first reception pipe, and the mixing of first alcohol and water is added in second reception pipe
Object dissolves the extract in two reception pipes；
E) by after the solution filtering in first reception pipe, filtered fluid is examined using gas chromatography tandem mass spectrometry method
It surveys；After the solution filtering in second reception pipe, filtered fluid is detected using Liquid Chromatography-Tandem Mass Spectrometry.
Wherein, in step a), the extracting solution is the mixed liquor of acetic acid and acetonitrile, wherein, the volume ratio of acetic acid and acetonitrile
It is 0.1~1:100.
Wherein, in step a), the mass ratio of the vegetables and fruits sample and the sodium chloride is 10：3~5.
Wherein, in step b), the mass ratio of the anhydrous magnesium sulfate and the extracting solution is not more than 1：10.
Wherein, it in step d), the supernatant liquor that is pipetted in first reception pipe and is pipetted in second reception pipe
The volume ratio of supernatant liquor is 3~5：1.
Wherein, in step d), the liquid in two reception pipes is dried up using nitrogen.
Wherein, in step d), in the mixture, the volume ratio of first alcohol and water is 3~4：7.
Wherein, in step e), using nylon filter film in the liquid in first reception pipe or second reception pipe
Liquid be filtered.
Wherein, in step a), mixed method uses vortex mixed method.
An embodiment of the present invention provides Multiple Pesticides method for detecting residue in a kind of vegetables and fruits, are purifying extracted vegetables and fruits agriculture
During residual extracting solution, by by extracting solution add in equipped with anhydrous magnesium sulfate, PSA and C18 fillers purification pipe in, vortex mixed pass through from
After heart processing, the extracting solution after being purified compared to existing purification method, does not need to, using Solid Phase Extraction column purification, subtract
The complexity of operating procedure is lacked, has reduced the time it takes in purification process, so as to improve the residual detection effect of vegetables and fruits agriculture
Rate, and the residual rate of recovery of higher agriculture can be obtained.
Description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, to embodiment or will show below
There is attached drawing needed in technology description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention, for those of ordinary skill in the art, without creative efforts, can be with
Other attached drawings are obtained according to these attached drawings.
Fig. 1 be acetonitrile as extracting solution when obtained by extract liquor chromatogram；
Fig. 2 be ethyl acetate as extracting solution when obtained by extract liquor chromatogram；
Fig. 3 be acetone as extracting solution when obtained by extract liquor chromatogram；
Fig. 4 is the schematic diagram of the Multiple Pesticides rate of recovery under different acetic acid, acetonitrile volume ratio；
Fig. 5 is schematic diagram of the different extraction times to the Multiple Pesticides rate of recovery；
Fig. 6 is to the schematic diagram of the Multiple Pesticides rate of recovery under different filling mixture ratio relationships.
Specific embodiment
Below in conjunction with the attached drawing in the embodiment of the present invention, the technical solution in the embodiment of the present invention is carried out clear, complete
Site preparation describes, it is clear that described embodiment is only part of the embodiment of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, those of ordinary skill in the art are obtained every other without creative efforts
Embodiment shall fall within the protection scope of the present invention.
Pesticides Testing method in existing vegetable and fruit, generally use gas chromatography-mass spectrography and liquid chromatography-tandem matter
Spectrometry establishes pesticide multi-residue determination method in vegetable and fruit with reference to gas (liquid) phase chromatograph-mass spectrometer coupling technology.It needs before detection
It extracts and purifies the pesticide residue in vegetables and fruits, generally by Solid Phase Extraction column purification, this purification method is usually will extraction
Liquid is transferred to column and component is made to be retained on column, by constantly eluting removal chaff interferent, then will be tested with the solvent of small size
Substance is eluted and is collected, it is seen that its operating process is complicated, and method critical control point is more, when causing purification cost more
Between, reduce whole detection efficiency.
An embodiment of the present invention provides Multiple Pesticides method for detecting residue in a kind of vegetables and fruits, may comprise steps of：
A) extracting solution is added in vegetables and fruits sample, after mixing, 10~30min of oscillation treatment adds sodium chloride, then
It is secondary to be centrifuged handling after mixing, obtain stratified liquid up and down.
In the present invention, vegetables and fruits sample can be selected from a part for vegetables or fruit, for example, the blade of vegetables, stem,
Root, the positions such as pericarp, the fruit of fruit.
In the present invention, extracting solution is generally organic solvent, for extracting the pesticide residue in vegetables and fruits, for pesticide residue
Extraction, be pesticide multi-residues detection method antecedent basis.The total requirement of extractant is Selective dissolution quilt as far as possible
Object and its metabolite are surveyed, and does not dissolve or dissolves matrix and impurity chaff interferent less.Therefore, consider tested pesticide polarity,
The factors such as selectivity and extractant boiling point, toxicity in extraction, distribution, purification process, the more residuals extraction being commonly used
Solvent is taken to have acetonitrile, acetone, ethyl acetate, these three extracting solutions can obtain the higher rate of recovery and the selection of wider pesticide
Range.As shown in Figure 1 to Figure 3, the chromatogram of gained extract liquor when respectively acetonitrile, ethyl acetate and acetone are as extracting solution.
In the present invention, acetonitrile, acetone, ethyl acetate can be used to be extracted as extracting solution to sample, three can
Meet rate of recovery requirement, but the extraction impurity of ethyl acetate and acetone is more, color is deep, and impurity peaks are more on chromatogram,
It is preferred that acetonitrile is selected as extracting solution.
For different vegetable, fruit matrix, pH value is different, and certain pesticides are very sensitive to acid-base value, as captan,
Can different degrees of degradation occur in alkaline environment for Bravo, dicofol etc., it is therefore desirable to adjust the pH value of extracting solution.
In the present invention, acetic acid may be used to be adjusted, the volume ratio with acetonitrile is 0.1~1:100.Fig. 4 is different acetic acid, acetonitrile
The schematic diagram of the Multiple Pesticides rate of recovery under volume ratio, as shown in figure 4, working as acetic acid：Acetonitrile volume ratio is 0.5:100 and 1:When 100,
Extracting solution is close to the above-mentioned recovery rate to soda acid sensitivity pesticide, but is apparently higher than pure acetonitrile system.In view of extracting solution system
In acid to chromatographic system work stability and durability degree have an impact, can be preferably 0.5 by the volume ratio of acetic acid and acetonitrile
~1:100.
In the present invention, concussion extraction time can be 5~30min, it is contemplated that shake the length of extraction time to tested
The extraction of object has different degrees of influence, and the extraction time for choosing 5min, 10min, 20min, 30min respectively is measured.With
More than solution ratio extracts, i.e., the volume ratio of acetic acid and acetonitrile is 0.5:When 100.As shown in figure 5, the quilt after 10min
It surveys the object rate of recovery and disclosure satisfy that requirement substantially, rate of recovery difference is little after extraction time is 10min, can keep stablizing.It is comprehensive
It closes and selects 20min as extraction Best Times after considering stability and conventional efficient.
Preferably, in above-mentioned steps a), vortex mixed method can be selected to mix reagent, so as to mix mixture
More uniformly.
B) anhydrous magnesium sulfate, PSA and C18 fillers are added in pipe is purified, wherein, anhydrous magnesium sulfate, PSA (N- propyl second
Diamines) volume ratio between C18 fillers is 4：1~3：3~1, obtain the purification pipe equipped with filler.
In the present invention, the filler purified in pipe can include：Anhydrous magnesium sulfate, PSA and C18.It removes in extracting solution
Water can improve the extraction efficiency of polarity pesticide in acetonitrile extracting solution, and can reduce polar impurity and chaff interferent in extracting solution.
Anhydrous magnesium sulfate has 3 times higher than anhydrous sodium sulfate of water absorbing capacity, has higher dehydration energy in processing sample as dehydrating agent
Power, so as to which acetonitrile is made more effectively to extract the pesticide in vegetables and fruits；PSA can effectively eliminate various organic acids, pigment and one
A little sugar and aliphatic acid；C18 has good clean-up effect to the nonpolarity such as grease in extracting solution and low pole impurity.
It should be noted that the small-sized centrifuge tube of 10mL may be used in the purification pipe in the present invention, it can realize and load this hair
Bright filler, the present invention is herein without limiting.
In the present invention, to reach enough dehydrating effects, extracting solution can be less than 10 with anhydrous magnesium sulfate mass ratio:1,
Dehydrating agent can be 1 with cleanser mass ratio:1.Wherein, for the overwhelming majority for acetonitrile, when 20 degrees Celsius of acetonitrile, is close in extracting solution
It spends for 0.982g/mL, therefore 1ml acetonitriles are approximately equal to 1g.Based on conditions above, 3 kinds of purification filler schemes, anhydrous sulphur can be chosen
Sour magnesium：PSA：C18 proportion relations can be respectively 4：1：3；4：2：2；4：3：1, and measure time of pesticide in the case of three kinds of proportionings
Yield as shown in fig. 6, the first proportion relation and second of proportion relation rate of recovery situation are essentially identical, but is matched at the third
The rate of recovery than acid agrichemicals several under relation condition is relatively low.It is final excellent in view of PSA to the clean-up effect of pigment, aliphatic acid
Select anhydrous magnesium sulfate：PSA：C18 proportion relations are 4：2：2.
C) supernatant liquor of liquid obtained by step a) is pipetted into the purification pipe equipped with filler, 1~2min of vortex mixed,
After being centrifuged processing, stratified liquid up and down is obtained.
Inventor the study found that directly the supernatant liquor of gained liquid can be pipetted into the purification pipe equipped with filler,
After vortex mixed and centrifuging treatment, stratified liquid up and down is obtained, so as to complete the purification of extracting solution, without that will carry
Liquid is taken the complexity of purifying step while clean-up effect is ensured, can be reduced, using Solid Phase Extraction column purification so as to subtract
The time it takes in few purification process, and then improve detection efficiency.It establishes a kind of suitable for high-throughput multi-pesticide residue screening detection
Method has very high application value and long-range application prospect.
D) supernatant liquor in the stratified liquid up and down for obtaining step c) is pipetted respectively into two reception pipes, and respectively
Drying, obtains extract, n-hexane is added in first reception pipe, and the mixing of first alcohol and water is added in second reception pipe
Object dissolves the extract in two reception pipes.
In the present invention, nitrogen at normal temperatures stablize by chemical property, is not susceptible to react, it is preferred that may be used
Nitrogen dries up the liquid in two reception pipes.
In the present invention, the supernatant liquor pipetted in first reception pipe and the upper strata pipetted in second reception pipe
The volume ratio of clear liquid can be 3~5：1；The supernatant liquor and the volume ratio of n-hexane pipetted in first reception pipe can be 4
~5：1；In second reception pipe, the volume ratio of first alcohol and water can be 3~4：7, the upper strata pipetted in second reception pipe is clear
The volume ratio of liquid and mixture can be 1：1~2.
E) by after the solution filtering in first reception pipe, filtered fluid is examined using gas chromatography tandem mass spectrometry method
It surveys；After the solution filtering in second reception pipe, filtered fluid is detected using Liquid Chromatography-Tandem Mass Spectrometry.
In the present invention, nylon filter film may be used in the liquid in first reception pipe or second reception pipe
Liquid be filtered, so as to filter out the large particulate matter in liquid.
In the present invention, mass spectrum used can be tandem mass spectrum.MS/MS (mass spectrum/mass spectrum) technology can be reduced or be disappeared
Except the interference of object unrelated in sample substrate, MS1 and MS2 is monitored by selection, can effectively reduce local noise interference, very big
Detection sensitivity is improved in degree, becomes the preferred method of trace detection.
The volume ratio of acetic acid and acetonitrile is used in the present invention as 0.1~1:100, it is remained as Multiple Pesticides in vegetable and fruit
The extracting solution of detection method in reasonably extraction liquid proportional and under the conditions of rational extraction time, can ensure hundreds of various agricultures
The extraction efficiency of medicine.Using rational proportion of filler, effective purification has been carried out to extracting solution.Use gas/liquid phase chromatography-series connection matter
The detection means of spectrum ensure that testing result accurately and reliably, can be effectively used for the remaining screening inspection of Multiple Pesticides in vegetable and fruit
It surveys.
Technical scheme of the present invention is described below in conjunction with specific embodiment, described embodiment is only this
Invention part of the embodiment, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art exist
All other embodiments obtained under the premise of creative work are not made, shall fall within the protection scope of the present invention.
Embodiment 1
Experiment reagent
Acetonitrile：Chromatographically pure；N-hexane：Chromatographically pure；Formic acid：Chromatographically pure；Acetic acid：It analyzes pure；Sodium chloride：It analyzes pure；It is anhydrous
Magnesium sulfate：It analyzes pure；PSA fillers；C18 fillers.
Laboratory apparatus
Gas chromatography tandem mass spectrometry instrument Agilent7890-7000, Liquid Chromatography-Tandem Mass Spectrometry instrument Waters Xevo TQ,
Electronic balance METTLER PL303, electric agitator IKA KS501, turbine mixer VORTEX-2, nitrogen evaporator Pu Litaike
EVA50A, centrifuge Hitachi CR 21G.
Detection process
Vegetables and fruits sample 200g is weighed, is smashed to pieces in bruisher, mixing, is preserved in 0~4 DEG C of refrigerator.Weigh the examination of 5.00g vegetables and fruits
Sample adds in 10mL extracting solutions in vegetables and fruits sample, and after vortex mixed is uniform, mechanical shaking extraction 20min adds 2g sodium chloride, then
After secondary vortex mixed is uniform, 20000r/min centrifugal treating 3min obtain the liquid of lower leaf, wherein, extracting solution is acetic acid
With the mixed liquor of acetonitrile, the volume ratio of acetic acid and acetonitrile is 0.5:100；Added in pipe is purified 400mg anhydrous magnesium sulfates,
200mg PSA and 200mg C18 fillers obtain the purification pipe equipped with filler；The supernatant liquor 7mL of gained liquid is measured to being equipped with
In the purification pipe of filler, vortex mixed 1min after being centrifuged processing, obtains stratified liquid up and down；By upper and lower stratified liquid
In supernatant liquor pipetted respectively into two reception pipes, first reception pipe 4mL, second reception pipe 1mL, and use nitrogen respectively
Air-blowing is done, and obtains extract, in first reception pipe add in 1mL n-hexanes, in second reception pipe add in 1mL methanol and
The mixture of water, the volume ratio of first alcohol and water is 4：7, dissolve the extract in two reception pipes；It will be in first reception pipe
Solution filtering after, filtered fluid is detected using gas chromatography tandem mass spectrometry method；By the solution mistake in second reception pipe
After filter, filtered fluid is detected using Liquid Chromatography-Tandem Mass Spectrometry.
Detection parameters are set：
GC conditions：
GC conditions are：Post case program：60 DEG C of holding 1min, are then warming up to 170 DEG C, then with every for 40 DEG C per minute
10 DEG C of minute is warming up to 310 DEG C, keeps 3min；Preceding injector：10μl；Sample size：1μl；Carrier gas：He, purity 99.999%；It carries
Gas velocity：1.0mL/min；Chromatographic column：350 DEG C of DB-5ms, MAX, 30m × 0.25mm × 0.25 μm；Transmission line temperature：280
℃。
Makings condition：
EI energy：70eV；Ion source temperature：300℃；Level four bars temperature：180℃；Solvent delay：4min.
Liquid phase chromatogram condition：
Sample size：5μl；；Flow velocity：0.4mL/min；Chromatographic column：Waters Auquity UPLC BEH C18,100mm ×
2.1mm×1.7μm。
Embodiment 2
It is using experiment reagent same as Example 1, laboratory apparatus, vegetables and fruits sample and detection parameters, detection process：
5.00g vegetables and fruits samples are weighed, 10mL extracting solutions, after vortex mixed is uniform, mechanical shaking extraction are added in vegetables and fruits sample
5min adds 1.5g sodium chloride, is vortexed again for after mixing, and 20000r/min centrifugal treating 3min obtain lower leaf
Liquid, wherein, mixed liquor of the extracting solution for acetic acid and acetonitrile, the volume ratio of acetic acid and acetonitrile is 0.1:100；In pipe is purified
400mg anhydrous magnesium sulfates, 300mg PSA and 100mg C18 fillers are added in, obtains the purification pipe equipped with filler；Measure gained liquid
In the supernatant liquor 7mL of body to the purification pipe equipped with filler, vortex mixed 1.5min after being centrifuged processing, is obtained up and down
Stratified liquid；Supernatant liquor in upper and lower stratified liquid is pipetted respectively into two reception pipes, first reception pipe 3mL, the
Two reception pipe 1mL, and being dried up respectively with nitrogen, obtain extract, and 1mL n-hexanes are added in first reception pipe, the
The mixture of 1mL first alcohol and waters is added in two reception pipes, the volume ratio of first alcohol and water is 3.5：7, make in two reception pipes
Extract dissolves；After the solution filtering in first reception pipe, filtered fluid is examined using gas chromatography tandem mass spectrometry method
It surveys；After the solution filtering in second reception pipe, filtered fluid is detected using Liquid Chromatography-Tandem Mass Spectrometry.
Embodiment 3
It is using experiment reagent same as Example 1, laboratory apparatus, vegetables and fruits sample and detection parameters, detection process：
5.00g vegetables and fruits samples are weighed, 10mL extracting solutions, after vortex mixed is uniform, mechanical shaking extraction are added in vegetables and fruits sample
30min adds 2.5g sodium chloride, is vortexed again for after mixing, and 20000r/min centrifugal treating 3min obtain lower leaf
Liquid, wherein, mixed liquor of the extracting solution for acetic acid and acetonitrile, the volume ratio of acetic acid and acetonitrile is 1:100；In purification Guan Zhongjia
Enter 400mg anhydrous magnesium sulfates, 100mg PSA and 300mg C18 fillers, obtain the purification pipe equipped with filler；Measure gained liquid
Supernatant liquor 7mL to equipped with filler purification pipe in, vortex mixed 2min after being centrifuged processing, obtains lower leaf
Liquid；Supernatant liquor in upper and lower stratified liquid is pipetted respectively into two reception pipes, first reception pipe 5mL, second
Reception pipe 1mL, and dried up respectively with nitrogen, extract is obtained, 1mL n-hexanes are added in first reception pipe, at second
The mixture of 1mL first alcohol and waters is added in reception pipe, the volume ratio of first alcohol and water is 4：7, make the extract in two reception pipes
Dissolving；After the solution filtering in first reception pipe, filtered fluid is detected using gas chromatography tandem mass spectrometry method；It will
After solution filtering in second reception pipe, filtered fluid is detected using Liquid Chromatography-Tandem Mass Spectrometry.
Multiple Pesticides method for detecting residue in a kind of vegetables and fruits provided by the present invention is described in detail above.Herein
In apply specific embodiment the principle of the present invention and embodiment be expounded, the explanation of above example is only intended to
It helps to understand method and its central idea of the invention.It should be pointed out that it for those of ordinary skill in the art, is not taking off
Under the premise of from the principle of the invention, can also to the present invention, some improvement and modification can also be carried out, these improvement and modification also fall into this
The protection of invention claim.
It should be noted that herein, term " comprising " or its any other variant are intended to nonexcludability
Comprising so that process, method, article or equipment including a series of elements are not only including those elements, but also wrap
Include other elements that are not explicitly listed or further include for this process, method, article or equipment it is intrinsic will
Element.In the absence of more restrictions, the element limited by sentence "including a ...", it is not excluded that wanted including described
Also there are other identical elements in the process of element, method, article or equipment.
Each embodiment in this specification is described using relevant mode, identical similar portion between each embodiment
Point just to refer each other, and the highlights of each of the examples are difference from other examples.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the scope of the present invention.It is all
Any modification, equivalent replacement, improvement and so within the spirit and principles in the present invention, are all contained in protection scope of the present invention
It is interior.
Claims (9)
1. a kind of Multiple Pesticides method for detecting residue in vegetables and fruits, which is characterized in that including：
A) extracting solution is added in vegetables and fruits sample, after mixing, 5~30min of mechanical shaking extraction adds sodium chloride, mixes again
After closing uniformly, it is centrifuged handling, obtains the liquid of lower leaf；
B) anhydrous magnesium sulfate, PSA and C18 fillers are added in pipe is purified, wherein, the volume between anhydrous magnesium sulfate, PSA and C18
Than being 4：1~3：3~1, obtain the purification pipe equipped with filler；
C) supernatant liquor of liquid obtained by step a) is pipetted into the purification pipe equipped with filler, 1~2min of vortex mixed, through from
After heart separating treatment, stratified liquid up and down is obtained；
D) supernatant liquor in the stratified liquid up and down for obtaining step c) is pipetted respectively into two reception pipes, and blow respectively
It is dry, extract is obtained, n-hexane is added in first reception pipe, the mixing of first alcohol and water is added in second reception pipe
Object dissolves the extract in two reception pipes；
E) by after the solution filtering in first reception pipe, filtered fluid is detected using gas chromatography tandem mass spectrometry method；It will
After solution filtering in second reception pipe, filtered fluid is detected using Liquid Chromatography-Tandem Mass Spectrometry.
2. Multiple Pesticides method for detecting residue in vegetables and fruits according to claim 1, which is characterized in that described in step a)
Extracting solution is the mixed liquor of acetic acid and acetonitrile, wherein, the volume ratio of acetic acid and acetonitrile is 0.1~1:100.
3. Multiple Pesticides method for detecting residue in vegetables and fruits according to claim 1 or 2, which is characterized in that in step a), institute
The mass ratio for stating vegetables and fruits sample and the sodium chloride is 10：3~5.
4. Multiple Pesticides method for detecting residue in vegetables and fruits according to claim 1, which is characterized in that described in step b)
The mass ratio of anhydrous magnesium sulfate and the extracting solution is not more than 1：10.
5. Multiple Pesticides method for detecting residue in vegetables and fruits according to claim 1, which is characterized in that in step d),
The supernatant liquor pipetted in one reception pipe and the volume ratio of supernatant liquor pipetted in second reception pipe are 3~5：1.
6. Multiple Pesticides method for detecting residue in vegetables and fruits according to claim 1 or 5, which is characterized in that in step d), adopt
The liquid in two reception pipes is dried up with nitrogen.
7. Multiple Pesticides method for detecting residue in vegetables and fruits according to claim 1 or 5, which is characterized in that in step d), institute
It states in mixture, the volume ratio of first alcohol and water is 3~4：7.
8. Multiple Pesticides method for detecting residue in vegetables and fruits according to claim 1, which is characterized in that in step e), use
Nylon filter film is filtered the liquid in first reception pipe or the liquid in second reception pipe.
9. Multiple Pesticides method for detecting residue in vegetables and fruits according to claim 1, which is characterized in that in step a), mixing
Method uses vortex mixed method.
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Cited By (4)
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| CN110057928A (en) * | 2019-02-27 | 2019-07-26 | 中国热带农业科学院农产品加工研究所 | A kind of ultra performance liquid chromatography tandem mass spectrometry detecting captan residual quantity in tomato |
| CN110361478A (en) * | 2019-08-13 | 2019-10-22 | 深圳市深大检测有限公司 | The detection method of remains of pesticide in a kind of vegetable and fruit |
| CN113109471A (en) * | 2021-04-12 | 2021-07-13 | 诺安实力可商品检验（青岛）有限公司 | LCMSMS (liquid crystal display module medium) method for rapidly and simultaneously detecting chlorothalonil and metabolites thereof in vegetables and fruits |
| CN114487224A (en) * | 2022-01-20 | 2022-05-13 | 中国农业科学院农业质量标准与检测技术研究所 | Method for detecting acidic pesticide in fruits and vegetables |
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