CN102252889A - Microwave-assisted solvent-free solid-phase headspace extraction device and extraction method thereof - Google Patents
Microwave-assisted solvent-free solid-phase headspace extraction device and extraction method thereof Download PDFInfo
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Abstract
The invention discloses a microwave-assisted solvent-free solid-phase headspace extraction device and an extraction method thereof. The device uses microwave for heating while a metering input pump is also used for extracting the air in a container continuously, the maximum extraction can be fast performed without using an organic solvent, the resource can be saved, and the environment can not be polluted; when the device is used for extracting volatile and semi-volatile components in a solid sample, microwave additives are selectively added into an extraction container according to the condition that the sample components absorb microwaves, the device is convenient and flexible; and the gaseous extract extracted by the device can be condensed to generate volatile oil, and then the related separation analysis is carried out on the volatile oil, or the volatile oil is directly introduced into a gaseous phase analytical instrument so as to be subjected to separation analysis such as gas chromatography, mass spectrum and ion mobility spectrometry. The method can be used for extracting the volatile and semi-volatile components in complex samples such as fresh plants, soil, traditional Chinese medicines building materials and the like.
Description
Technical field
The present invention relates to compartment analysis field, particularly the pretreating device of volatile constituent compartment analysis and method in the solid sample to component in the complex sample.
Background technology
For the compartment analysis of component in the complex sample, the sample pre-treatments particularly extraction of effective constituent is unusual critical step.Normal at present employing solvent extraction method such as water vapour extraction, Soxhlet extraction etc. utilize dissolving power and/or component the distribution capability in solvent and matrix of component in solvent to realize extracting.In leaching process,, often need to use a large amount of organic solvents because the dissolving of solvent and distribution saturability are the maximum extraction that realizes component in the sample.A large amount of uses of solvent cause the bigger environmental pollution and the wasting of resources.In addition, solvent extraction method also exists to extract uses duration, usually the time spent of sample extraction and pre-treatment the over half of whole analysis time spent that account for, extract poor selectivity, some components easily produce chemical changes such as decomposition, reaction in leaching process, extract solvent and put forward the deficiencies such as later separation analysis generation interference of the existence of thing to component to be measured altogether.
Microwave energy is a kind of electromagenetic wave radiation, can penetrate sample interior, and sample integral body is heated, and has even heating, the characteristics of no thermograde.The dipole molecule that microwave heating is based in sample and/or the solvent produces effects such as dipole eddy current, ionic conduction and high-frequency friction under the effect of microwave energy, produce a large amount of heats at short notice.Because microwave heating has characteristics such as quick, efficient, energy-conservation, even heating, has been widely used in fields such as production, life, scientific research at present.
It is one of microwave energy important application in sample pre-treatments that microwave-assisted extracts, and is a kind of cleaning extractive technique that the time spent is short, extraction ratio is high, safe, fast, efficient that extracts.Microwave-assisted be extracted in volatile ingredient in the complex samples such as Chinese crude drug, soil, food extract in existing a large amount of research and application reports.Existing microwave-assisted extracts need use a large amount of solvents, similar with solvent extraction method, has environmental pollution, solvent equally and carry thing altogether may produce deficiencies such as chemical change to component to be measured in the follow-up compartment analysis generation interference of component to be measured, the leaching process.
The solvent-free extraction of microwave-assisted is to extract development on the basis and next a kind of novel extracting method at microwave-assisted, thereby utilize microwave heating to make component to be measured be converted into the principle realization extraction that gaseous state separates from matrix, have characteristics such as safe, fast, efficient, pollution-free.The solvent-free extraction of microwave-assisted need not with an organic solvent, is a kind of extracting method of environmental protection and energy saving, is specially adapted to the extraction of volatility and half volatile component in the sample.Difficult volatile constituent is difficult to be converted into gaseous state in the sample, so be not extracted out, therefore the follow-up compartment analysis of component to be measured disturbs few.In addition, the solvent-free extraction of microwave-assisted is a kind of head space extractive technique, is equivalent to use air to be extraction agent.Similar with the solvent in the solvent extraction method, air exists the distribution saturated phenomenon equally.And along with gaseous state volatile constituent constantly overflowing from the extraction system, air in the extraction system also is carried the system of leaving simultaneously, in the i.e. extraction system air along with the Microwave Extraction process carry out fewer and fewerily, influenced the extraction of the extraction of subsequent component, particularly high boiling component.In order farthest to extract volatility and the half volatile component, particularly high boiling component in the sample, need to bring in constant renewal in ozone, play being similar to the effect that solvent upgrades in the Soxhlet extraction, and existing extraction element all can not satisfy this point.
At above-mentioned deficiency, need to explore a kind of microwave-assisted solvent-free solid phase head space extraction element and extracting method, make it can bring in constant renewal in extraction agent (air) in the extraction system, efficiently, extract volatility and half volatile component in the sample apace, particularly high boiling component is avoided the interference of other coexistence component in the complex sample simultaneously.
Summary of the invention
In view of this, the invention provides a kind of microwave-assisted solvent-free solid phase head space extraction element and extracting method thereof, reach the air that to bring in constant renewal in the extraction system and extract volatility in the sample efficiently, apace and the purpose of half volatile component.
The solvent-free solid phase head space of microwave-assisted of the present invention extraction element, comprise microwave heating equipment and be arranged at the interior extraction vessel of microwave heating equipment, be communicated with respectively on the described extraction vessel and be provided with intake line and output pipe, the intake line front end is provided with the metering front pump.
Further, described intake line and output pipe are made by high temperature resistant teflon, polyetheretherketone or Kynoar;
Further, the entry position of described output pipe is higher than the exit position of intake line;
Further, described metering front pump is an injecting type metering front pump.
The present invention also provides a kind of method of utilizing the solvent-free solid phase head space of above-mentioned microwave-assisted extraction element to extract volatile constituent in the solid sample, this method is: component absorbs the situation of microwave property per sample, selectively in extraction vessel, add one or more potpourri in carbonyl iron dust, dag and the activated carbon powder as the microwave auxiliary agent, if sample itself contains moisture or component to be measured has polarity, then can not add any microwave auxiliary agent.
Beneficial effect of the present invention: the solvent-free solid phase head space of microwave-assisted of the present invention extraction element utilizes microwave heating, can bring in constant renewal in air in the extraction vessel by the metering front pump simultaneously, need not with an organic solvent can farthest extract apace, economize on resources, free from environmental pollution, when using this device that the volatility in the solid sample and half volatile component are extracted, component absorbs the situation of microwave property per sample, selectively in extraction vessel, add the microwave auxiliary agent, convenient, flexible, this device extracts the condensable back of the gaseous state extract that obtains and obtains the volatile oil compartment analysis of being correlated with again, also can be directly connected to and carry out compartment analysis in the gas phase analysis instrument, as gas chromatograph, mass spectrum, Ion mobility spectrometry etc.This method can be used for as the volatility in the complex samples such as fresh plant, soil, Chinese crude drug, gypsum, sheet material, building materials, the extraction of half volatile component.
Description of drawings
Below in conjunction with drawings and Examples the present invention is further described.
Fig. 1 is a structural representation of the present invention;
Fig. 2 is the gas chromatography compartment analysis spectrogram of Chinese crude drug curcuma zedoary volatile constituent after the present invention extracts.
Embodiment
Fig. 1 is a structural representation of the present invention, Fig. 2 is the gas chromatography compartment analysis spectrogram of Chinese crude drug curcuma zedoary volatile constituent after the present invention extracts, as shown in the figure: the solvent-free solid phase head space of the microwave-assisted of present embodiment extraction element, comprise microwave heating equipment 1 and the extraction vessel 2 that is arranged in the microwave heating equipment 1, be communicated with respectively on the described extraction vessel 2 and be provided with intake line 3 and output pipe 4, intake line 3 front ends are provided with metering front pump 5, utilize microwave heating that volatilization and half volatile component in the solid sample are gasified, can bring in constant renewal in air in the extraction vessel by the metering front pump simultaneously, need not with an organic solvent can farthest extract apace, economize on resources, free from environmental pollution.
In the present embodiment, described intake line 3 and output pipe 4 are made by teflon, polyetheretherketone or Kynoar, and resistance to elevated temperatures is good.
In the present embodiment, the entry position of described output pipe 4 is higher than the exit position of intake line 3, helps the even distribution of extraction agent (air) in sample bottle, farthest to carry away the gaseous component after the microwave gasification.
In the present embodiment, described metering front pump 5 is injecting type metering front pump, and implementation cost is lower, and the injecting type front pump is provided with volume markings, is easy to the air capacity that quantitatively control is upgraded.
Utilize the solvent-free solid phase head space of above-mentioned microwave-assisted extraction element to extract the method for volatile constituent in the solid sample, component absorbs the situation of microwave property per sample, selectively in extraction vessel 2, add carbonyl iron dust as the microwave auxiliary agent, if sample itself contains moisture or component to be measured has polarity, then can not add any microwave auxiliary agent, adopt the microwave auxiliary agent to help maximum extraction.Certainly, the potpourri of one or more in employing carbonyl iron dust, dag and the activated carbon powder all can be realized purpose of the present invention.
Use above-mentioned microwave-assisted solvent-free solid phase head space extraction element and extracting method that the Chinese crude drug curcuma zedoary is extracted the back gas chromatographic analysis:
Microwave Extraction: the Chinese crude drug curcuma zedoary is shredded into fine particulate, take by weighing 3.0g, place the 50mL conical flask, connect in the solvent-free solid phase head space of the microwave-assisted device, the setting microwave power is 800W, opens microwave heating equipment, heating 4min, the extraction agent syringe pump injects air 2mL.The volatile constituent of the curcuma zedoary Chinese crude drug that extracts through the six-way valve sample introduction, is directly carried out the gas chromatography compartment analysis.
GC analyzes: gas chromatograph, be furnished with flame ionization ditector (FID), chromatographic column be the AC-5 fused-silica capillary column (30m * 320 μ m, 0.25 μ m, SGE), the HW-2000 chromatographic work station.Column temperature: 60 ℃ of initial temperatures, keep 3min, rise to 80 ℃ with 3 ℃/min, keep 1min, rise to 180 ℃ with 5 ℃/min, keep 1min, rise to 220 ℃ with 10 ℃/min, keep 3min.Fid detector: 250 ℃; Carrier gas is high purity nitrogen (purity 〉=99.999%), and flow velocity 1.5mL/min does not shunt.
Measurement result is as shown in Figure 2: curcuma zedoary is the dry rhizome of turmeric section plant zedoary, Guangxi zedoary and RADIX CURCUMAE, its principal ingredient is sesquiterpenoids and sesquiterpene compounds, comprise rcumenol, curdione, germacrone, australene, nopinene, elemene etc., have effects such as antitumor, antiviral, antibiotic, anti-inflammatory, treatment epilepsy, clinical practice is extensive.Adopt the gaseous state volatile constituent after the solvent-free solid phase head space of microwave-assisted extracts directly to carry out the capillary gas chromatography compartment analysis, go out peak number above 50, contained volatile constituent is more in the gained presentation of results curcuma zedoary, and basic, normal, high boiling point component all can well go out the peak.
The extraction that the solvent-free solid phase head space of microwave-assisted among the present invention extraction element is not limited to the volatility in the solid matrix, half volatile component separates, and the extraction that also can be used for volatility, half volatile component in the wet samples such as water body, blood separates.
Explanation is at last, above embodiment is only unrestricted in order to technical scheme of the present invention to be described, although the present invention is had been described in detail with reference to preferred embodiment, those of ordinary skill in the art is to be understood that, can make amendment or be equal to replacement technical scheme of the present invention, and not breaking away from the aim and the scope of technical solution of the present invention, it all should be encompassed in the middle of the claim scope of the present invention.
Claims (5)
1. the solvent-free solid phase head space of microwave-assisted extraction element, it is characterized in that: comprise microwave heating equipment (1) and be arranged at the interior extraction vessel (2) of microwave heating equipment (1), be communicated with respectively on the described extraction vessel (2) and be provided with intake line (3) and output pipe (4), intake line (3) front end is provided with and measures front pump (5).
2. the solvent-free solid phase head space of microwave-assisted according to claim 1 extraction element is characterized in that: described intake line (3) and output pipe (4) are made by high temperature resistant teflon, polyetheretherketone or Kynoar.
3. the solvent-free solid phase head space of microwave-assisted according to claim 1 and 2 extraction element is characterized in that: the entry position of described output pipe (4) is higher than the exit position of intake line (3).
4. the solvent-free solid phase head space of microwave-assisted according to claim 1 and 2 extraction element is characterized in that: described metering front pump (5) is injecting type metering front pump.
5. method of using any solvent-free solid phase head space of the described microwave-assisted extraction element of claim 1-4 to extract volatile constituent in the solid sample, it is characterized in that: component absorbs the situation of microwave property per sample, selectively in extraction vessel (2), add one or more potpourri in carbonyl iron dust, dag and the activated carbon powder as the microwave auxiliary agent, if sample itself contains moisture or component to be measured has polarity, then can not add any microwave auxiliary agent.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105617711A (en) * | 2014-10-16 | 2016-06-01 | 中国药科大学 | New technology for separating trace components in complex sample through combination of a class of magnetic ionic liquids and corresponding micro-extraction apparatus |
| CN108949363A (en) * | 2018-09-26 | 2018-12-07 | 常德华馥生物技术有限公司 | A kind of Solventless Extraction Process of industrial hemp floral leaf essential oil |
| CN110022873A (en) * | 2016-12-01 | 2019-07-16 | 自然萃取系统有限责任公司 | Utilize the quick-speed plant oil distilling apparatus of microwave agent |
| CN111983097A (en) * | 2020-08-28 | 2020-11-24 | 中国农业科学院油料作物研究所 | Microwave extraction method for two-dimensional gas quality detection of volatile substances in edible oil |
| CN112126523A (en) * | 2020-09-22 | 2020-12-25 | 漳州职业技术学院 | Plant essential oil extraction device and extraction method |
| CN112620329A (en) * | 2020-11-30 | 2021-04-09 | 桂林电子科技大学 | Soil organic matter pollution treatment device |
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| CN200958099Y (en) * | 2006-09-26 | 2007-10-10 | 汤大卫 | Essence extractor |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105617711A (en) * | 2014-10-16 | 2016-06-01 | 中国药科大学 | New technology for separating trace components in complex sample through combination of a class of magnetic ionic liquids and corresponding micro-extraction apparatus |
| CN105617711B (en) * | 2014-10-16 | 2018-04-10 | 中国药科大学 | A kind of magnetic ionic liquids combine related micro-extraction device and are used for microcomponent separation method in complex sample |
| CN110022873A (en) * | 2016-12-01 | 2019-07-16 | 自然萃取系统有限责任公司 | Utilize the quick-speed plant oil distilling apparatus of microwave agent |
| CN108949363A (en) * | 2018-09-26 | 2018-12-07 | 常德华馥生物技术有限公司 | A kind of Solventless Extraction Process of industrial hemp floral leaf essential oil |
| CN111983097A (en) * | 2020-08-28 | 2020-11-24 | 中国农业科学院油料作物研究所 | Microwave extraction method for two-dimensional gas quality detection of volatile substances in edible oil |
| CN112126523A (en) * | 2020-09-22 | 2020-12-25 | 漳州职业技术学院 | Plant essential oil extraction device and extraction method |
| CN112620329A (en) * | 2020-11-30 | 2021-04-09 | 桂林电子科技大学 | Soil organic matter pollution treatment device |
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Application publication date: 20111123 |