CN108176365A - It is a kind of for the solid absorbent materials and preparation method of QuEChERS methods and application - Google Patents
It is a kind of for the solid absorbent materials and preparation method of QuEChERS methods and application Download PDFInfo
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Abstract
The present invention relates to a kind of solid absorbent materials for QuEChERS methods and preparation method and applications.The solid absorbent materials are prepared to include the following steps：1) after carbon material is completely dissolved in organic solvent, modified silica-gel material and catalyst are added in it, then at a temperature of being placed in 40~60 DEG C, reacts 20~28h, take solids；2) solids made from step 1) is added in hydrazine hydrate solution, then at a temperature of being placed in 85~105 DEG C, after reacting 1.5~2.5h, take solid to get.When solid absorbent materials of the present invention are applied to improve QuEChERS methods, suitable for a variety of matrix, the remaining detection and analysis of Multiple Pesticides.The solid absorbent materials are cheap, and step is simple, are easy to obtained.Its adsorption capacity is moderate, ensures the rate of recovery of analyte in sample.Processing procedure is easy to operate, and analysis time is short, while improves precision of analysis.
Description
Technical field
The invention belongs to analytical chemistry fields, and in particular to a kind of solid absorbent materials for QuEChERS methods and its
Preparation method and application.
Background technology
For raising grain yield, meet population increasing need, and the pest and disease damage influence in farmland also tends to cause
The crops underproduction significantly, therefore, various chemical pesticides would have to be used by large area, and the thing followed is inevitable
Pesticide Residue.Health of the pesticide residue concerning people is one of most important part in food-safety problem, in order to
Strengthen the monitoring and management of pesticide residue, exploitation is easy, quick, accurately detection method is very important.
QuEChERS methods are one based on acetonitrile liquid-liquid extraction, anhydrous MgSO4Saltout layering, brothers amine dispersed solid phase extraction
Take the quick sample pretreatment method of three steps of purification.QuEChERS methods are because of it with simple and efficient, safe and reliable etc. all
More advantages by the continuous improvement and optimized development, have been widely used in various fields, especially Detecting Pesticide point
Analysis.
For QuEChERS methods in purification process, the sorbing material used has ethylenediamine base-N- propyl silanes, C18, graphite
Alkene and graphitized carbon etc., because pesticide variety is various, sample substrate type is various, and property is there is also difference, and pesticide is often
Be it is a variety of be used together, therefore for pesticide multi-residues sample processing still there are some defects, such as part pesticide
Adsorb it is too strong, fraction matrix can not reduce interference etc., the rate of recovery is caused to reduce, influence method detection limit and accuracy.Therefore, it seeks
Look for the purifying adsorbent that a kind of property is more excellent, Multiple Pesticides residual, a variety of matrix samples is suitble to handle extremely important.
Invention content
First of the present invention is designed to provide a kind of good solid absorbent materials of the clean-up effect to various samples
Preparation method.Especially for the sample of higher, the acid special natures such as stronger of lipid content, clean-up effect is apparent.
The preparation method includes the following steps：
1) after carbon material is completely dissolved in organic solvent, modified silica-gel material and catalyst are added in, then be placed in it
At a temperature of 40~60 DEG C, 20~28h is reacted, takes solids；
2) solids made from step 1) is added in hydrazine hydrate solution, then at a temperature of being placed in 85~105 DEG C, reaction
After 1.5~2.5h, solid is taken to get the solid absorbent materials.
Present invention further propose that, the carbon material is graphene oxide or graphene；Preferably graphene oxide.
The organic solvent is selected from N,N-dimethylformamide, dichloromethane, acetonitrile.Preferably N,N-dimethylformamide
Present invention further propose that, the modified silica-gel material is bonded silane (PSA) for ethylenediamine-N- propyl；
The mass ratio of the carbon material and the modified silica-gel material is 5:20~30, preferably 5:23~27；Most preferably
It is 5:25.
Present invention further propose that, the catalyst is selected from dicyclohexylcarbodiimide (DCC), 1- (3- dimethylaminos
Propyl) -3- ethyl-carbodiimide hydrochlorides/I-hydroxybenzotriazole (EDCI/HOBT), one in N, N '-carbonyl dimidazoles (CDI)
Kind is a variety of；
Preferably dicyclohexylcarbodiimide.
The mass ratio of the carbon material and the catalyst is 5:0.5~2, preferably 5:0.8~1.2, most preferably 5:
1。
Present invention further propose that, the molar concentration of hydrazine hydrate is 0.15~0.2mol/L in the hydrazine hydrate solution；
Preferably 0.17~0.18mol/L.
Commercially available to arrive the hydrazine hydrate that hydrazine hydrate is 85%, it is 85 that described 85% hydrazine hydrate, which is mass ratio,:100 hydration
The mixed liquor of hydrazine and water.
Every gram of solids adds the hydrazine hydrate solution of 20~30mL；Preferably every gram of solids addition 24
The hydrazine hydrate solution of~26mL.
Present invention further propose that, carbon material is completely dissolved in organic solvent and is specially in step 1)：By carbon material plus
Enter in organic solvent, with 12~17min of power ultrasonic of 80~120w.
Present invention further propose that, after step 1) takes after solids and takes solid in step 2), further include washing,
Dry, dispersion；
Wherein, the washing is successively using water and methanol, alternatively, water and ethyl alcohol carry out；Preferably water and methanol.
The drying is 50~70 DEG C；The drying is preferably using drying.
The dispersion is specially：The solid is slightly ground, its sheet is made to scatter.
The solid absorbent materials are characterized using AFM, SEM, IR and XPS, and characterization result can be participated in following specific
Embodiment.
The present invention provides a kind of preferred embodiment, and the preparation method of the solid absorbent materials includes the following steps：
1) graphene oxide is completely dissolved in n,N-Dimethylformamide, then is added in and graphene oxide quality to it
Than being 5:23~27:0.8~1.2 ethylenediamine-N- propyl bonding silane and dicyclohexylcarbodiimide, is placed in 45~55 DEG C
At a temperature of, after reacting 22~26h, take solids, washing, drying；
2) solids made from step 1) is added in hydrazine hydrate solution, then at a temperature of being placed in 90~100 DEG C, reaction
After 1.8~2.2h, take solid, washing, it is dry, grind to get；
The molar concentration of hydrazine hydrate is 0.17~0.18mol/L in the hydrazine hydrate solution；
Every gram of solids adds the hydrazine hydrate solution of 24~26mL.
It is a second object of the invention to provide solid absorbent materials made from any of the above-described preparation method.
It is a third object of the invention to provide the solid absorbent materials obtained by any preparation method are in QuEChERS side
Application in method.
The QuEChERS methods specifically comprise the following steps：
1) homogenate is made in sample to be tested, internal standard is added in it13C- hexachloro-benzenes after standing 3~8min, add extraction
Agent and anhydrous magnesium sulfate and sodium chloride；With frequency 3~8min of vortex oscillation of 2000~3000r/min, then with 4500~
5500r/min rotating speeds centrifuge 4~6min, take extract liquor；
The mass ratio of the homogenate, the anhydrous magnesium sulfate and the sodium chloride is 8~12:3~5:1；
2) in the extract liquor of step 2), anhydrous magnesium sulfate and any solid phase adsorption material of claim 1~8 are added in
Expect, after shaken well, centrifugation takes supernatant；
3) supernatant is subjected to gas-chromatography-Tandem Mass Spectrometry Analysis.
Present invention further propose that, the QuEChERS methods specifically comprise the following steps：
1) homogenate is made in sample to be tested, internal standard is added in it13C- hexachloro-benzenes after standing 3~8min, add second
Nitrile and anhydrous magnesium sulfate and sodium chloride；With 4~6min of hunting of frequency of 2300~2700r/min, then with 4500~5500r/
Min rotating speeds centrifuge 4~6min, take extract liquor；
The mass ratio of the homogenate, the anhydrous magnesium sulfate and the sodium chloride is 10:4:1；
2) 1mL is taken out in the extract liquor of step 2), adds in anhydrous magnesium sulfate and any solid phase of claim 1~8
Sorbing material, after shaken well, centrifugation takes supernatant；
The anhydrous magnesium sulfate is 5~7 with the solid absorbent materials mass ratio:1；The nothing is added in per 1mL extract liquors
140~160mg of the water magnesium sulfate and solid absorbent materials 24-26mg.
3) after the supernatant to be crossed to 0.2 μm of film, gas-chromatography-Tandem Mass Spectrometry Analysis is carried out.
Preferably, every gram of homogenate uses the acetonitrile of 0.8~1.2mL.
Solid absorbent materials of the present invention combine traditional material ethylenediamine-N- propyl bonding silane and graphene
Advantage, applied to improve QuEChERS methods when, suitable for a variety of matrix, the remaining detection and analysis of Multiple Pesticides.Described consolidates
Phase sorbing material is cheap, and step is simple, is easy to obtained.Its adsorption capacity is moderate, ensures the rate of recovery of analyte in sample.
Processing procedure is easy to operate, and analysis time is short, while improves precision of analysis.
Description of the drawings
Fig. 1 is the preparation principle figure of solid absorbent materials described in embodiment 1；
Fig. 2 is that the AFM of solid absorbent materials described in embodiment 1 characterizes collection of illustrative plates；
Fig. 3 is that the SEM of solid absorbent materials described in embodiment 1 characterizes collection of illustrative plates；
Fig. 4 is that the IR of solid absorbent materials described in embodiment 1 characterizes collection of illustrative plates；
Fig. 5 is that the XPS of solid absorbent materials described in embodiment 1 characterizes collection of illustrative plates；
Total ion currents of the Fig. 6 for 67 kinds of pesticide mark-ons in celery sample measured by the QuEChERS methods described in embodiment 4
Figure；
Fig. 7 be eaten measured by the QuEChERS methods described in embodiment 5 in cowpea sample 67 kinds of pesticide mark-ons always from
Subflow figure；
Fig. 8 is solid absorbent materials described in embodiment 1, C18, graphene and ketjenblack EC difference scavenging material
The total ion current figure comparison of 67 kinds of pesticide mark-ons in cowpea sample measured by QuEChERS methods；
Fig. 9 is solid absorbent materials described in embodiment 1, C18, graphene and ketjenblack EC difference scavenging material
The rate of recovery comparison of part pesticide in cowpea sample measured by QuEChERS methods；
Figure 10 is cowpea sample measured by the QuEChERS methods of the solid absorbent materials described in Examples 1 to 3 and comparative example 1
Part pesticide peak type figure compares in product.
Specific embodiment
The following examples are used to illustrate the present invention, but are not intended to limit the scope of the present invention..
Embodiment 1
The present embodiment provides a kind of preparation methods of solid absorbent materials, include the following steps：
1) graphene oxide of 0.5g is added in the n,N-Dimethylformamide of 150mL, at the power ultrasonic of 100W
Manage 15min；Silane and the dicyclohexylcarbodiimide (DCC) of 0.1g are bonded with the ethylenediamine-N- propyl of 2.5g to its addition again,
At a temperature of being placed in 50 DEG C, fully after reaction for 24 hours, decompression filters, and collects solids, and water and methanol wash 3 times successively, dries；
2) solids made from taking 2g steps 1) is added in the hydrazine hydrate solution of 50.5mL, then at a temperature of being placed in 95 DEG C,
After reacting 2h, solid is taken, after water washing 3 times, then washed 3 times using methanol, drying, grinding distribution is to get solid absorbent materials；
Wherein, the molar concentration of hydrazine hydrate is 0.17~0.18mol/L in the hydrazine hydrate solution.
Obtained solid absorbent materials are characterized using AFM, SEM, IR and XPS, reference can be made to Fig. 2~5.
Embodiment 2
The present embodiment provides a kind of preparation methods of solid absorbent materials, include the following steps：
1) graphene of 0.5g is added in the n,N-Dimethylformamide of 150mL, is handled with the power ultrasonic of 100W
15min；Silane and the dicyclohexylcarbodiimide of 0.1g are bonded with the ethylenediamine-N- propyl of 2.5g to its addition again, is placed in 50
At a temperature of DEG C, fully after reaction for 24 hours, decompression filters, and collects solids, after water washing 3 times, then is washed 3 times using methanol, dried
It is dry；
2) solids made from taking 2g steps 1) is added in the hydrazine hydrate solution of 50.5mL, then at a temperature of being placed in 95 DEG C,
After reacting 2h, solid is taken, after water washing 3 times, then washed 3 times using methanol, drying is ground to get solid absorbent materials；
Wherein, the molar concentration of hydrazine hydrate is 0.17~0.18mol/L in the hydrazine hydrate solution.
Embodiment 3
The present embodiment provides a kind of preparation methods of solid absorbent materials, include the following steps：
1) graphene oxide of 0.5g is added in the n,N-Dimethylformamide of 150mL, at the power ultrasonic of 100W
Manage 15min；Silane and the N of 0.1g, N '-carbonyl dimidazoles (CDI) are bonded with the ethylenediamine-N- propyl of 2.5g to its addition again,
At a temperature of being placed in 50 DEG C, fully after reaction for 24 hours, decompression filters, and collects solids, after water washing 3 times, then is washed using methanol
3 times；
2) solids made from taking 2g steps 1) is added in the hydrazine hydrate solution of 50.5mL, then at a temperature of being placed in 95 DEG C,
After reacting 2h, solid is taken, after water washing 3 times, then washed 3 times using methanol, drying is ground to get solid absorbent materials；
Wherein, the molar concentration of hydrazine hydrate is 0.17~0.18mol/L in the hydrazine hydrate solution.
Embodiment 4
The present embodiment utilizes solid absorbent materials described in embodiment 1, using QuEChERS methods, to pesticide in celery
Residual is detected, and is specifically comprised the following steps：
1) homogenate is made in celery sample to be tested, takes 10g, the internal standard of 0.05mg is added in the homogenate as described in every 1kg, to
Internal standard is added in the homogenate13C- hexachloro-benzenes after standing 3~8min, add 10mL acetonitriles, are shaken with miniature vortex mixed instrument
After swinging the frequency vortex oscillation 1min with 2500r/min, 4g anhydrous magnesium sulfates and 1g sodium chloride are added；After persistent oscillation 4min,
5min is centrifuged with 5000r/min rotating speeds, takes extract liquor；
2) the extract liquor 1mL that step 2) is taken to obtain, adds in 150mg anhydrous magnesium sulfates and 25mg solid absorbent materials, use are micro-
Type vortex mixed instrument vibrates, and centrifugation takes supernatant；
3) after the supernatant that step 2) is obtained to be crossed to 0.2 μm of film, gas-chromatography-Tandem Mass Spectrometry Analysis is carried out.
Embodiment 5
The present embodiment is using the solid absorbent materials obtained by embodiment 1, using QuEChERS methods, to cowpea middle peasant
Medicine residual is detected, and is specifically comprised the following steps：
1) homogenate is made in cowpea sample to be tested, takes 10g, the internal standard of 0.05mg is added in the homogenate as described in every 1kg, to
It adds in internal standard13C- hexachloro-benzenes after standing 3~8min, add 10mL acetonitriles, are vibrated with miniature vortex mixed instrument with 2500r/
After the frequency vortex oscillation 1min of min, 4g anhydrous magnesium sulfates and 1g sodium chloride are added；After persistent oscillation 4min, with 5000r/min
Rotating speed centrifuges 5min, takes extract liquor；
2) the extract liquor 1mL that step 2) is taken to obtain, adds in 150mg anhydrous magnesium sulfates and 25mg solid absorbent materials, use are micro-
Type vortex mixed instrument vibrates, and centrifugation takes supernatant；
3) after the supernatant that step 2) is obtained to be crossed to 0.2 μm of film, gas-chromatography-Tandem Mass Spectrometry Analysis is carried out.
Comparative example 1
This comparative example provides a kind of preparation method of solid absorbent materials, with differing only in for embodiment 1：In step 2)
Add in the hydrazine hydrate solution of 40.5mL.
Test example 1
Pesticide residue in cowpea is detected using QuEChERS methods；Method and step is same
Embodiment 5.
Wherein, pesticide variety includes five classes：Organic phosphates, organochlorine class, chrysanthemum esters, carbamates and triazines
Herbicide.
Solid absorbent materials described in embodiment 1 (PSA@G), C is respectively adopted in solid absorbent materials18(C18), graphene
(G) and ketjenblack EC (GCB).
As a result it compares：
1st, the total ion current figure of 67 kinds of pesticide mark-ons is compared referring to Fig. 8 in measured cowpea sample.As shown in Figure 8：With C18、
Graphene compares with graphitized carbon, and solid absorbent materials clean-up effect described in embodiment 1 is best, using described in embodiment 1
The obtained result peak type of solid absorbent materials purified treatment it is best, interference is minimum.
2nd, the rate of recovery of part pesticide is compared referring to Fig. 9 in measured cowpea sample.
In five class pesticides are surveyed, one or two kinds of representative species progress rate of recovery comparative analyses are chosen per a kind of：Chlordene
Benzene (Hexachlorobenzene), carbofuran (carbofuran), Atrazine (Atrazine), chlopyrifos
(Chlorpyrifos), DDE-p, p ', Biphenthrin (Bifenthrin).The results are shown in Figure 9：Due to graphene and and graphite
Changing carbon, this kind of coplanar pesticide has stronger adsorption capacity to hexachloro-benzene, causes the rate of recovery relatively low, it is impossible to meet testing requirements,
Especially for carbofuran (Carbofuran).Other three classes scavenging material C18, graphene and graphitized carbon all show it is relatively strong
Matrix effect, and solid absorbent materials described in embodiment 1 are then to the matrix effect of whole pesticides than relatively low, and the rate of recovery
Well, therefore solid absorbent materials described in embodiment 1 are best purification material.
Test example 2
Pesticide residue in cowpea is detected using QuEChERS methods；Wherein, reality is respectively adopted in solid phase adsorption discretion
Apply example 1~3 and the solid absorbent materials described in comparative example 1.Method and step is the same as embodiment 5.Clean-up effect comparison is as shown in Figure 10：
By taking the spectrogram of secbumeton (secbumeton) as an example, wherein, 1-1~1-4 distinguishes corresponding embodiment 2, embodiment left to bottom right
3rd, embodiment 1, peak type spectrogram obtained by solid absorbent materials described in comparative example 1.
As seen from the figure, minimum is interfered using the spectrogram that solid absorbent materials described in embodiment 1 obtain, peak type symmetry is most
It is good.
Although above having used general explanation, specific embodiment and experiment, the present invention is made to retouch in detail
It states, but on the basis of the present invention, it can be made some modifications or improvements, this is apparent to those skilled in the art
's.Therefore, these modifications or improvements without departing from theon the basis of the spirit of the present invention, belong to claimed
Range.
Claims (10)
1. the preparation method of a kind of solid absorbent materials for QuEChERS methods, which is characterized in that include the following steps：
1) after carbon material is completely dissolved in organic solvent, modified silica-gel material and catalyst are added in it, then it is placed in 40~
20~28h is reacted at a temperature of 60 DEG C, takes solids；
2) solids made from step 1) is added in hydrazine hydrate solution, then reaction 1.5 at a temperature of being placed in 85~105 DEG C~
After 2.5h, solid is taken to get the solid absorbent materials.
2. preparation method according to claim 1, which is characterized in that the carbon material is graphene oxide or graphene；
And/or the organic solvent is one or more in n,N-Dimethylformamide, dichloromethane, acetonitrile.
3. preparation method according to claim 1 or 2, which is characterized in that the modified silica-gel material is ethylenediamine-N- third
Base is bonded silane；
Preferably, the mass ratio of the carbon material and the modified silica-gel material is 5:20~30.
4. according to any preparation method of claims 1 to 3, which is characterized in that the catalyst is selected from dicyclohexyl carbon
Diimine, 1- (3- dimethylamino-propyls) -3- ethyl-carbodiimide hydrochlorides/I-hydroxybenzotriazole, N, N '-carbonyl dimidazoles
In it is one or more；
Preferably, the mass ratio of the carbon material and the catalyst is 5:0.5~2.
5. according to any preparation method of Claims 1 to 4, which is characterized in that hydrazine hydrate in the hydrazine hydrate solution
Molar concentration is 0.15~0.2mol/L；Every gram of solids adds the hydrazine hydrate solution of 20~30mL；
Preferably, the molar concentration for stating hydrazine hydrate in hydrazine hydrate solution is 0.17~0.18mol/L；Every gram of solids
Add the hydrazine hydrate solution of 24~26mL.
6. according to any preparation method of Claims 1 to 5, which is characterized in that taken in step 1) after solids and step
2) after taking solid in, washing, drying, dispersion are further included；
Preferably, the washing is successively using water and methanol, alternatively, water and ethyl alcohol carry out；
And/or the temperature of the drying is 50~70 DEG C；
And/or the dispersion is specially：The solid is slightly ground to sheet dispersion.
7. preparation method according to claim 1, which is characterized in that include the following steps：
1) graphene oxide is completely dissolved in n,N-Dimethylformamide, then is with graphene oxide mass ratio to its addition
5:23~27:0.8~1.2 ethylenediamine-N- propyl bonding silane and dicyclohexylcarbodiimide is placed in 45~55 DEG C of temperature
Under, after reacting 22~26h, take solids, washing, drying；
2) solids made from step 1) is added in hydrazine hydrate solution, then at a temperature of being placed in 90~100 DEG C, reaction 1.8~
After 2.2h, take solid, washing, it is dry, disperse to get；
The molar concentration of hydrazine hydrate is 0.17~0.18mol/L in the hydrazine hydrate solution；
Every gram of solids adds the hydrazine hydrate solution of 24~26mL.
8. the solid absorbent materials obtained by any preparation method of claim 1~7.
9. the solid absorbent materials or solid phase according to any one of claims 8 obtained by any preparation method of claim 1~7 are inhaled
Application of the enclosure material in QuEChERS methods, which is characterized in that the QuEChERS methods specifically comprise the following steps：
1) homogenate is made in sample to be tested, internal standard is added in it13C- hexachloro-benzenes after standing 3~8min, add extractant,
And anhydrous magnesium sulfate and sodium chloride；With 2300~2700r/min frequency 3~8min of vortex oscillation, then with 4500~5500r/
Min rotating speeds centrifuge 4~6min, take extract liquor；
The mass ratio of the homogenate, the anhydrous magnesium sulfate and the sodium chloride is 8~12:3~5:1；
2) in the extract liquor of step 2), anhydrous magnesium sulfate and any solid absorbent materials of claim 1~8 is added in, are shaken
After swinging uniformly, centrifugation takes supernatant；
3) supernatant is subjected to gas-chromatography-Tandem Mass Spectrometry Analysis.
10. application according to claim 9, which is characterized in that the QuEChERS methods specifically comprise the following steps：
1) homogenate is made in sample to be tested, internal standard is added in it13C- hexachloro-benzenes after standing 3~8min, add acetonitrile, with
And anhydrous magnesium sulfate and sodium chloride；With frequency 4~6min of vortex oscillation of 2300~2700r/min, then with 4500~5500r/
Min rotating speeds centrifuge 4~6min, take extract liquor；
The mass ratio of the homogenate, the anhydrous magnesium sulfate and the sodium chloride is 10:4:1；
2) 1mL is taken out in the extract liquor of step 2), adds in anhydrous magnesium sulfate and any solid phase adsorption of claim 1~8
Material, after shaken well, centrifugation takes supernatant；
The anhydrous magnesium sulfate is 5~7 with the solid absorbent materials mass ratio:1；The anhydrous sulphur is added in per 1mL extract liquors
Sour 140~160mg of the magnesium and 24~26mg of solid absorbent materials；
3) after the supernatant to be crossed to 0.2 μm of film, gas-chromatography-Tandem Mass Spectrometry Analysis is carried out.
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| CN111435128A (en) * | 2020-04-03 | 2020-07-21 | 宁波市疾病预防控制中心 | Method for measuring 4 diester-type aconite alkaloids in blood |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111435128A (en) * | 2020-04-03 | 2020-07-21 | 宁波市疾病预防控制中心 | Method for measuring 4 diester-type aconite alkaloids in blood |
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Application publication date: 20180619 |