CN205352813U - Multi -functional airtight microwave extraction device - Google Patents
Multi -functional airtight microwave extraction device Download PDFInfo
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- CN205352813U CN205352813U CN201620019434.0U CN201620019434U CN205352813U CN 205352813 U CN205352813 U CN 205352813U CN 201620019434 U CN201620019434 U CN 201620019434U CN 205352813 U CN205352813 U CN 205352813U
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Abstract
The utility model relates to a multi -functional airtight microwave extraction device, it includes: the jar body (4), its opening is sealed through sealed fill up (2) by upper cover (3), sample containing barrel hangs set (5), and it is the ring structure and sets up on the inner wall of the jar body (4) or become the integrated design with the inner wall of the jar body (4), sample containing barrel (7), it is the open drum structure in both ends, and its top has the outward flange in order to support on sample containing barrel hung set (5), its bottom had the inward flange and supports perforated sieve board (12) on this inward flange.
Description
Technical field
This utility model belongs to analytical chemistry sample pre-treatments field, is specifically related to a kind of multifunctional airtight microwave extracting apparatus, it is adaptable to organic extraction and purification in the field samples such as biology, food, environment, chemical industry, pharmacy.
Background technology
Microwave extracting due to high efficiency, strong selectivity, easy and simple to handle, by-product is few and productivity advantages of higher is widely used in fields such as environment, food, industry, natural product and Chinese medicines.Microwave extracting system can be divided into uncovered gerotor type and the big class of enclosed high pressure formula two according to extractor type.Its middle and high voltage type is then heated solvent and be immersed in sample therein in high-pressure bottle, and target components is extracted from sample matrices by solvent at high temperature under high pressure.In high-pressure microwave extraction process, the existence of pressure makes solvent be easier to enter in cell or sample space and discharge target components, is conducive to the mass transfer of target components to spread, compares uncovered gerotor type microwave extracting in hgher efficiency.But target components and interference impurity are extracted in extractant simultaneously, so that the steps such as extra purification, filtration just can detect.This makes the pre-treatment step of sample detection complicated and tediously long, and shifts sample between each step and can cause the loss of sample size.
Solid phase extraction techniques is to utilize solid-phase adsorbent the target components in fluid sample to be adsorbed, and makes target components and sample matrices and interference magazins' layout, then eluting or desorbing again, reaches to separate and be enriched with the purpose of target compound.Solid-Phase Extraction has response rate height, solvent consumption is few, easy and simple to handle, be prone to the advantages such as automatization, has been used for environment, food, biology, medicine and other fields at present.But Solid-Phase Extraction there is also open defect, as can not be directly processed solid sample, poor repeatability, sample etc. can not being processed in a large number.
Utility model content
This utility model is intended to overcome the defect that closed microwave extraction selectivity is poor, Solid-Phase Extraction can not directly process solid sample, devise a kind of multifunctional airtight microwave extracting apparatus, it is made to combine closed microwave extracting efficient quickly and the high advantage of Solid-Phase Extraction selectivity, simultaneously completed high pressure extraction, purified, dewatered, the step such as extract filtration, simplify operating procedure, reduce sample loss, improve preci-sion and accuracy.
This utility model is achieved through the following technical solutions:
A kind of multifunctional airtight microwave extracting apparatus, comprising:
Tank body 4, its opening is capped 3 and is sealed by sealing gasket 2；
Sample accommodation tube appending disk 5, it is circular ring structure and is arranged on the inwall of tank body 4 or designs with inwall integralization of tank body 4；
Sample accommodation tube 7, it is the cylindrical structure of both ends open, and its top has outward flange to be supported on described sample accommodation tube appending disk 5, and its bottom has inward flange and the porous sieve plate 12 being supported on this inward flange.
Preferably, have inside described sample accommodation tube 7 and dewatered oxidant layer 9 and sample layer 10 that adsorbent layer 11 is clipped in the middle.
Preferably, it is respectively provided with solvent circulation passage 6 on the top flange of sample accommodation tube 7 described in sample accommodation tube sample accommodation tube and on the annulus of described sample accommodation tube appending disk 5.Under in working order, these solvent circulation passages keep unimpeded.
Preferably, cover on described and be provided with pressure release orifice (1).
Preferably, between described porous sieve plate 12 and the diapire of described tank body 4, leave extractant hold space 8.Solvent level can lower than porous sieve plate 12, it is also possible to higher than porous sieve plate 12, it might even be possible to higher than the top of sample accommodation tube.But most preferably make solvent level lower than porous sieve plate 12.
According to a kind of multifunctional airtight microwave extracting apparatus of the present utility model, described tank body is made by the macromolecular material such as politef, sample accommodation tube by the macromolecular materials such as politef, Pyrex glass (Pyrex), quartzy, ceramic etc. make.
According to a kind of multifunctional airtight microwave extracting apparatus of the present utility model, described tank body internal diameter is 2～10cm, and tank body height is 5～20cm.
According to a kind of multifunctional airtight microwave extracting apparatus of the present utility model, described sample accommodation tube internal diameter is 1.5～9cm, is highly 1～10cm
According to a kind of multifunctional airtight microwave extracting apparatus of the present utility model, described sample accommodation tube and have solvent circulation passage on sample accommodation tube appending disk, its quantity is 1-100, and diameter is 1～10mm.
According to a kind of multifunctional airtight microwave extracting apparatus of the present utility model, described porous sieve plate can be made up of glass core, quartz core, pottery sieve plate, and its aperture is 1.5～50 μm.
This utility model also proposed a kind of use method carrying out closed microwave extraction according to above-mentioned multifunctional airtight microwave extracting apparatus, comprises the following steps:
(1) in tank body, extractant is added；
(2) sieve plate in sample accommodation tube is sequentially placed into adsorbent, sample and deicer；
(3) sample accommodation tube is put on sample accommodation tube appending disk, and make solvent circulation passage unimpeded；
(4) closed microwave extraction is carried out when making solvent seethe with excitement after airtight.
According to a kind of multifunctional airtight microwave assisted extraction methods that the utility model proposes, adsorbent on described sample accommodation tube, deicer, sample placement order do not limit with consumption.
According to a kind of multifunctional airtight microwave assisted extraction methods that the utility model proposes, described adsorbent at least includes one or more of: florisil silica class, diatom great soil group, silica type, alumina type, C18 class, graphitization carbons, resinae, and other organic or inorganic adsorbing material, nano materials.
According to a kind of multifunctional airtight microwave assisted extraction methods that the utility model proposes, described deicer at least includes one or more of: anhydrous sodium sulfate, anhydrous magnesium sulfate, anhydrous calcium chloride.
According to a kind of multifunctional airtight microwave assisted extraction methods that the utility model proposes, described extractant at least includes one or more of following organic solvent or reagent: methanol, ethanol, acetonitrile, acetone, ethyl acetate, dichloromethane, normal hexane, hexamethylene, pentane, normal heptane, toluene, water, soda acid buffer solution etc..
According to a kind of multifunctional airtight microwave extracting apparatus that the utility model proposes and method, can pesticide residues in extracted tobacco, it is not limited to this preferred embodiment, apply also for the method for organic extraction and purification in the field samples such as biology, food, environment, chemical industry, pharmacy.
Compared with prior art, it has the beneficial effect that this utility model
1) achieve high pressure extraction, purify, dewater, the step such as extract filtration carries out in a vessel simultaneously, simplifies operating procedure, reduces sample loss, improves preci-sion and accuracy.
2) extracting under high pressure and microwave radiation, mass transfer rate is fast, extracts and purification efficiency is high.
3) per sample and target components, different extractant, adsorbent, deicer can be selected, and sample load mode can independent assortment according to demand, have the wider suitability and range of application.
General introduction for technical solutions of the utility model described above, in order to be better understood upon technological means of the present utility model, and can be practiced according to the content of description, and in order to above-mentioned and other objects, features and advantages of the present utility model can be become apparent, now especially exemplified by preferred embodiment, and coordinate accompanying drawing, describe in detail as follows.
Accompanying drawing explanation
Fig. 1 is extractor schematic diagram；
Fig. 2 is the top view of sample accommodation tube appending disk 5；
Fig. 3 is the schematic diagram of sample accommodation tube 7；
Fig. 4 is the top view of sample accommodation tube 7；
Wherein, 1, pressure release orifice, 2 sealing gaskets, 3, upper cover, 4, tank body, 5, sample accommodation tube appending disk, 6, solvent circulation passage, 7, sample accommodation tube, 8, extractant hold space, 9, dewater oxidant layer, and 10, sample layer, 11, adsorbent layer, 12, porous sieve plate.
Fig. 5 and Fig. 6 is with florisil silica for adsorbent, anhydrous sodium sulfate is deicer, ethyl acetate-hexane (1:1, v/v) is extractant, uses above-mentioned multifunctional airtight microwave extracting apparatus to analyze the GC-TOFMS total ion current figure of 1.0g tobacco sample Pesticide Residues:
Wherein Fig. 5 is the total ion current figure of pestsides synthesis standard solution (0.1mg/L)；Fig. 6 is the total ion current figure of Nicotiana tabacum L. mark-on sample (25 μ g/kg).
In Fig. 5 and Fig. 6, the implication at each peak is as follows, and 1, Perchlorobenzene, 2, α-Gamma Hexaochlorocyclohexane, 3, gamma hch, 4, β-Gamma Hexaochlorocyclohexane, 5, heptachlor, 6, δ-Gamma Hexaochlorocyclohexane, 7, drinox, 8, trans-Niran, 9, cis-Niran, 10, dieldrin
Detailed description of the invention
Below in conjunction with embodiment, this utility model is described in further detail, but it is not limiting as this utility model.
As Figure 1-Figure 4, for the multifunctional airtight microwave extracting apparatus that the utility model proposes, comprising: tank body 4, upper cover 3, sealing gasket 2, pressure release orifice 1, sample accommodation tube appending disk 5, sample accommodation tube 7, solvent circulation passage 6, porous sieve plate 12, adsorbent layer 11, the oxidant layer that dewaters 9, sample layer 10.Their spatial relation as mentioned above and as it is shown in figure 1, repeats no more.
In closed microwave extraction process, tank body 4 adds extractant, put into sieve plate 12, adsorbent layer 11, sample layer 10 on sample accommodation tube 7, dewater oxidant layer 9, appropriateness compacting, the sample accommodation tube 7 loaded is put into tank body 4, and it is directed at solvent circulation passage 6, sealing gasket 2 is installed, after covering tightly upper cover 3, carries out closed microwave extraction.The extractant of bumping and the solvent vapo(u)r of generation enter in sample accommodation tube 7 by solvent circulation passage 6 and sieve plate 12, solvent is through sample 10, extract object and interference impurity, the adsorbed agent 11 of impurity is adsorbed, water is adsorbed by deicer 9, analyte is collected in extractant, thus reach to extract, purify, dewater, filter synchronous completes, last accommodation space 8 from extractant is sampled obtaining the solvent containing target components to be measured, it has already been through extraction, dewaters and remove impurity process, it is possible to be directly used in chromatographic isolation.Described tank body internal diameter is 2～10cm, and tank body height is 5～20cm.Described sample accommodation tube internal diameter is 1.5～9cm, is highly 1～10cm.Having solvent circulation passage on described sample accommodation tube and sample accommodation tube appending disk, its quantity is 1-100, and diameter is 1～10mm.Described sieve plate can be made up of glass core, quartz core, pottery sieve plate, and its aperture is 1.5～50 μm.Adsorbent layer on described sample accommodation tube, the oxidant layer that dewaters, sample layer placement order do not limit with consumption.Described adsorbent includes one or more of: florisil silica class, diatom great soil group, silica type, alumina type, C18 class, graphitization carbons, resinae, and other adsorbing materials, nano material.Described deicer includes one or more of: anhydrous sodium sulfate, anhydrous magnesium sulfate, anhydrous calcium chloride.Described extractant includes one or more of following organic solvent or reagent: methanol, ethanol, acetonitrile, acetone, ethyl acetate, dichloromethane, normal hexane, hexamethylene, pentane, normal heptane, toluene, water, soda acid buffer solution etc..
Embodiment: adopt multifunctional airtight microwave extracting apparatus to analyze the pesticide residues in Nicotiana tabacum L. in conjunction with gas chromatogram-flight time mass spectrum (GC-TOFMS).
Its concrete operations are: be 4cm at internal diameter, it is highly addition 60mL ethyl acetate-hexane (1:1 in the tank body of 15cm, v/v) extractant, it is 2.5cm at internal diameter, highly for the sample accommodation tube of 5cm is sequentially placed into glass core sieve plate that aperture is 30 μm, 2.0g florisil silica adsorbent, 1.0g sample, 0.5g anhydrous sodium sulfate deicer, appropriateness compacting, the sample accommodation tube loaded is put into tank body, and it is directed at solvent circulation passage, its quantity is 12, and diameter is 2.5mm.Sealing gasket is installed, puts into Microwave Extraction Apparatus after covering tightly upper cover and carry out closed microwave extraction, its microwave irradiation power 100W, extracting pressure 400kPa, extraction time 5min.
Table 1 is that multifunctional airtight microwave extracting apparatus analyzes the test data of the pesticide residues in Nicotiana tabacum L. in conjunction with gas chromatogram-flight time mass spectrum (GC-TOFMS).Table 1 gives the closed microwave extraction equipment/gas chromatogram-range of linearity of flight time mass spectrum combination analysis method, linearly dependent coefficient, precision (RSD), detection limit, quantitative limit and response rate relevant parameter, it was shown that the analysis detection of the pesticide residues that the method is suitable in Nicotiana tabacum L..
Table 1 range of linearity, linearly dependent coefficient, precision (RSD), detection limit, quantitative limit and the response rate
In the above-described embodiments, the application adopting Nicotiana tabacum L. Pesticide Residues to be object description multifunctional airtight microwave extracting apparatus.But this utility model is not limited only to this preferred application, by adopting the extractor of different volumes, the sample accommodation tube of different volumes, different adsorbents, deicer, extractant and suitable extraction parameters etc., could be applicable to organic extraction and purification in the field samples such as other biology, food, environment, chemical industry, pharmacy.
The above, be only preferred embodiment of the present utility model, and this utility model not does any pro forma restriction.Although this utility model illustrates as above with preferred embodiment, but it is not limited to this utility model, any those skilled in the art, without departing within the scope of technical solutions of the utility model, when the technology contents of available the disclosure above makes the Equivalent embodiments changing or modifying equivalent variations, in every case it is the content without departing from technical solutions of the utility model, any simple modification, equivalent variations and modification above example made according to technical spirit of the present utility model, all still falls within the scope of technical solutions of the utility model.
Claims (4)
1. a multifunctional airtight microwave extracting apparatus, it is characterised in that described multifunctional airtight microwave extracting apparatus includes:
Tank body (4), its opening is capped (3) and is sealed by sealing gasket (2)；
Sample accommodation tube appending disk (5), it is circular ring structure and is arranged on the inwall of tank body (4) or designs with inwall integralization of tank body (4)；
Sample accommodation tube (7), it is the cylindrical structure of both ends open, its top has outward flange to be supported on described sample accommodation tube appending disk (5), and its bottom has inward flange and the porous sieve plate (12) being supported on this inward flange.
2. multifunctional airtight microwave extracting apparatus according to claim 1, it is characterized in that, in described sample accommodation tube (7) inside, there is the sample layer (10) being clipped in the middle by the oxidant layer that dewaters (9) and adsorbent layer (11).
3. multifunctional airtight microwave extracting apparatus according to claim 1, it is characterized in that, on the top flange of described sample accommodation tube (7) and on the annulus of described sample accommodation tube appending disk (5), be respectively provided with solvent circulation passage (6).
4. multifunctional airtight microwave extracting apparatus according to claim 1, it is characterised in that leave extractant between the diapire of described porous sieve plate (12) and described tank body (4) and hold space (8).
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105527149A (en) * | 2016-01-11 | 2016-04-27 | 云南中烟工业有限责任公司 | Multifunctional closed microwave extraction device, and using method and purpose thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105527149A (en) * | 2016-01-11 | 2016-04-27 | 云南中烟工业有限责任公司 | Multifunctional closed microwave extraction device, and using method and purpose thereof |
| CN105527149B (en) * | 2016-01-11 | 2018-08-03 | 云南中烟工业有限责任公司 | A kind of multifunctional airtight microwave extracting apparatus, its application method and purposes |
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