CN102788722B - Organic pretreatment system for food samples - Google Patents
Organic pretreatment system for food samples Download PDFInfo
- Publication number
- CN102788722B CN102788722B CN201210297569.XA CN201210297569A CN102788722B CN 102788722 B CN102788722 B CN 102788722B CN 201210297569 A CN201210297569 A CN 201210297569A CN 102788722 B CN102788722 B CN 102788722B
- Authority
- CN
- China
- Prior art keywords
- extraction
- concentration
- module
- module comprises
- concentrated
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Landscapes
- Sampling And Sample Adjustment (AREA)
Abstract
The invention relates to an organic pretreatment system for food samples. The organic pretreatment system comprises an extraction module, a pre-concentration module, a purification module and a volume ensuring module. The extraction module comprises a high-pressure pump, a pressure-proof extraction and cleaning pool and a pressure and temperature control and protection valve unit and is used for extraction of the samples to obtain extract of a target compound. The pre-concentration module comprises a concentration cup, an infusion pump and a gas and liquid channel control valve unit and is used for concentration of the extract to obtain concentration liquid of the target compound. The purification module comprises an SPE (solid phase extraction) column and is used for purification of the concentration liquid to obtain purification liquid of the target compound. The volume ensuring module comprises a concentration cup, a cold trap, a vacuum pump and an infusion pump and is used for concentration and volume ensuring of the purification liquid. Under premise of guaranteeing organic pretreatment effect of the food samples, seamless connection between the samples to be detected and analyzing and detecting equipment is really achieved, unattended operation is achieved, and labor intensity of operators is reduced greatly.
Description
Technical field
The present invention relates to a kind of system for food safety detection sample pretreatment.
Background technology
Along with the develop rapidly of modern chemical analysis technology, analysis means is more and more towards quick, trace, accurate, automatic future development, and sample pre-treatments has become the technical bottleneck that restriction Modern Methods develops.
Food samples has comparatively complicated matrix (high grease, pigment, sugar etc.), in actual testing process, be prone to false positive and false-negative testing result, and the factor that causes accuracy reduction comes from the pre-treatment link of sample more, therefore the pre-treatment of food samples is particularly important especially.
Generally, the organic pre-treatment work of food samples mainly comprises extraction, pre-concentration, purification and the concentrated constant volume four processes of sample.For the extraction of food samples, in laboratory, there are soxhlet's extraction, ultrasonic extraction and the quick solvent extraction that in recent years just grown up at present; Concentration technique is mainly that the auxiliary nitrogen of heating blows concentrated and Vacuum Concentration; Purification techniques mainly contains Solid-Phase Extraction (SPE) technology and gel purification (GPC) technology.Solvent extraction technology is compared conventional art fast, can reduce the consumption of organic solvent, shortens extraction time, more easily realizes robotization, improves the reappearance of sample.Solid phase extraction techniques has good reappearance and treatment effeciency because of it, in assay laboratory, is used widely.But, existing pre-processing device has only been realized automation function in a certain link of food pre-treatment, and linking between link needs too much artificial participation, really realize to meaning the automatic, efficient of sample pre-treatments, simultaneously artificial participation has not only improved operator's labour intensity but also has increased the generation of artificial accidental error.
Summary of the invention
Technical matters solved by the invention is to provide a kind of organic preprocessing system of full-automatic food sample with extraction, pre-concentration, purification and constant volume function, solve the technical bottleneck problem of complicated loaded down with trivial details sample pretreatment in food safety detection, realize the Quick Pretreatment of food samples.
For reaching above-mentioned purpose, the technical solution used in the present invention is:
The organic preprocessing system of a kind of food samples, comprises extraction module, pre-concentration module, cleaning module and constant volume module; Described extraction module comprises high-pressure pump, withstand voltage extraction and service sink, pressure and temp control and protection valve group, completes sample extraction work, obtains the extract of target compound; Described pre-concentration module comprises that concentrated cup A, infusion pump A, gas-liquid road operation valve group and nitrogen blow enrichment facility, completes the concentrated work of above-mentioned extract, obtains the concentrate of target compound; Described cleaning module comprises Solid-Phase Extraction SPE post, completes the purification of above-mentioned concentrate, obtains the scavenging solution of target compound; Described constant volume module comprises concentrated cup B, cold-trap, vacuum pump and infusion pump B, completes the concentrated and constant volume of above-mentioned scavenging solution.
The organic preprocessing system of food samples of the present invention, wherein said extraction module comprises high-pressure pump, withstand voltage extraction and service sink, stream threeway, retaining valve, pressure unit, relief valve and stop valve; After described high-pressure pump, connect withstand voltage extraction and service sink by stream threeway; Another path is again by stream threeway Connection Release valve and pressure unit respectively; After pressure unit, connect retaining valve; Withstand voltage extraction is connected stop valve with after service sink.
The organic preprocessing system of food samples of the present invention, wherein said pre-concentration module comprises concentrated cup A, infusion pump A and is located at the stop valve of concentrated cup A lower end outlet, and emptying stop valve and nitrogen purge valve; Described concentrated cup A bottom is provided with liquid level sensor.
The robotization that the invention has the beneficial effects as follows supporting technologies such as having realized pressure extraction technology and concentrated, purification, constant volume is integrated, has realized all food samples, comprises the full-automatic Quick Pretreatment of solid and fluid sample.The present invention is ensureing under the prerequisite of the organic pre-treatment effect of food samples, can realize nearly automatically processing continuously of 24 samples, really realized the seamless link of testing sample and analyzing and testing equipment room, unmanned completely, has greatly reduced operator's labour intensity.In addition this invention also can expanded application in environmental sample as robotization sample pre-treatments such as soil, bed mud, water sample, solid waste.
Brief description of the drawings
Fig. 1 is the schematic diagram of the organic preprocessing system of food samples of the present invention;
Fig. 2 A is the schematic diagram of extraction module;
Fig. 2 B is the schematic diagram of pre-concentration module;
Fig. 2 C is the schematic diagram of cleaning module;
Fig. 2 D is the schematic diagram of constant volume module;
Wherein, 1: high-pressure pump; 2: extraction or clean pond; 3: concentrated cup A; 4: infusion pump A; 5:SPE post; 6: seal assembly; 7: infusion pump B; 8: concentrated cup B; 9:; Cold-trap; 10: vacuum pump; 11: pressure unit; 12: liquid level sensor.
Wherein, solid line represents liquid road; Dotted line represents gas circuit.
Embodiment
For further illustrating the present invention, illustrate with the following Examples:
As shown in Figure 1, the present invention is a kind of organic preprocessing system of full-automatic food sample with extraction, pre-concentration, purification and constant volume function, comprises the extraction module, pre-concentration module, cleaning module and the constant volume module that connect in turn; Extraction module comprises high-pressure pump 1, withstand voltage extraction and service sink 2, stream threeway, retaining valve, pressure unit 11, relief valve and stop valve; After described high-pressure pump 1, connect withstand voltage extraction and service sink 2 by stream threeway; Another path is again by stream threeway Connection Release valve and pressure unit 11 respectively; The rear connection retaining valve of pressure unit 11; The rear connection stop valve of withstand voltage extraction and service sink 2;
Pre-concentration module comprises concentrated cup A3, infusion pump A4 and is located at the stop valve of concentrated cup A3 lower end outlet, and emptying stop valve and nitrogen purge valve; Described concentrated cup A4 bottom is provided with liquid level sensor 12;
Cleaning module comprises Solid-Phase Extraction SPE post 5 and seal assembly 6;
Constant volume module comprises concentrated cup B8, cold-trap 9, vacuum pump 10 and infusion pump B7.
In use, first operator is quantitatively transferred to the sample after homogeneous withstand voltage extraction and service sink 2, at elevated pressures and temperature, complete fast extraction work, then by high pressure nitrogen, extract is purged to follow-up concentrated cup A, then extract nitrogen blowing in the situation that heating is auxiliary is concentrated, by nitrogen, concentrate and follow-up cleaning fluid are purged to successively on follow-up Solid-Phase Extraction SPE post 5 and complete wash-out more afterwards, extract after purification is collected in quantitatively concentrated cup B, heating in vacuum concentrates constant volume, so far completes the whole process of sample pre-treatments.
As shown in Figure 2 A, extraction module major function has been sample extraction work, obtains the extract of target compound.Described extraction module chief component comprises high-pressure pump, withstand voltage extraction and service sink (separately joining 25 rotating disks), stream threeway, retaining valve, pressure unit, relief valve and stop valve.25 above-mentioned rotating disks can carry 24 abstraction pools and 1 service sink and can realize the automatic switchover between pond.At work, first operator loads sample into abstraction pool, be placed on rotating disk, then walk abstraction pool is connected into extraction stream by system controlling software control rotating disk, now stop valve is closed, high-pressure pump starts, in abstraction pool, inject extraction solvent and pressure is added to default value (generally at 10Mpa ~ 15Mpa), then termination of pumping, start abstraction pool and carry heating function intensification heating abstraction pool (normal temperature ~ 200 ° C), because temperature control equipment is equipment well known to those skilled in the art, therefore be not repeated.Under certain temperature and pressure, keep a period of time the stripping of (>=5min) realize target compound.Afterwards, stop valve is opened, and high-pressure pump starts the sample rinsing in abstraction pool, finally adopts high pressure nitrogen that all extracts are purged to the concentrated cup into pre-concentration module, so far completes the extraction work of a sample.And then, walked service sink is connected into extraction stream by system controlling software control rotating disk, now stop valve is opened, and high-pressure pump starts, detergent line, and cleaning fluid is purged to above-mentioned concentrated cup by high pressure nitrogen in the lump.
Especially as shown in Figure 2 A, high-pressure pump, pressure unit and relief valve have formed the control pressurer system of extraction module, in extraction process, the pressure of pressure unit Real-Time Monitoring abstraction pool changes, if pressure surge lower than setting value 0.3Mpa high-pressure pump by automatic compensation, if pressure exceedes setting value 0.3Mpa, relief valve can carry out micro-release (micro updating), ensures the stability and security of instrument.
As shown in Figure 2 B, pre-concentration module comprises concentrated cup, infusion pump and gas-liquid road operation valve group, and gas circuit is marked by dotted line, and main fluid path indicated by solid line, and major function has been the concentrated work of extract, obtains the concentrate of target compound.This module adopts the concentrated pattern of the auxiliary nitrogen blowing of heating, realizes the concentrated of extract, is equipment well known to those skilled in the art, therefore be not repeated because nitrogen blows enrichment facility.At work, concentrated cup lower end outlet shutoff valve is given tacit consent in closed condition, after extract is transferred in concentrated cup completely, open emptying stop valve and nitrogen purge valve, concentrated cup carries heating jacket and can allow concentrated cup keep (being generally 60 ~ 70 ° of C) at a certain temperature simultaneously, utilizes nitrogen blowing concentrated extract.The liquid level sensor of concentrated cup bottom can detect extract liquid level, to prevent that extract from, by complete evaporate to dryness, causing the loss of target compound.After completing etc. concentrated work, outlet shutoff valve is opened, emptying stop valve is closed, utilize the pressure that nitrogen blows concentrate to be purged on the SPE post of cleaning module, as shown in Figure 2 C, then infusion pump delivery solvent is cleaned concentrated cup and is utilized the pressure that nitrogen blows cleaning fluid to be purged on the SPE post of cleaning module, and infusion pump pumps into solvent wash-out SPE post under nitrogen pressure afterwards, flow out scavenging solution, so far completed the purification work of concentrate.
Especially as shown in Figure 2 B, the online concentrated pattern of design employing of concentrated module, concentrated cup adopts two-way Parallel Design, and two-way control switching is controlled by two-position three-way valve.At work, by being used alternatingly of two the concentrated streams in left and right, can realize the continuous concentration of multiple sample extraction liquid.Lift an example, in the time that operator extracts the 1st sample, two-way pre-concentration cup is all in vacant state, when the 1st sample extraction completes, extract is transferred to the concentrated work that starts extract after the concentrated cup in the left side, at the same time, extraction module starts the extraction work of the 2nd sample, switch and make the right concentrated cup stream be communicated with extraction module the extract of preparing to receive the 2nd sample by two-bit triplet, after the 2nd sample extraction completes, the concentrated cup in the right is collected the extract of the 2nd sample and is started to heat nitrogen and blows concentrated, at this moment the concentrated cup in the left side the 2nd sample extraction during this period of time in completed the concentrated of the 1st sample, before the extract that receives the 3rd sample, automatically discharge the concentrate of the 1st sample and complete cleaning, pass through SPE post what discharge cleaning solvent, as shown in Figure 2 C, can complete the purification of the concentrate of the 1st sample simultaneously, and then in the time completing the extraction work of the 3rd sample, complete pre-concentration and the purification of the 2nd sample extraction liquid, in this way repeatedly, can realize the parallel processing that extraction and pre-concentration purify, save working time of nearly sixty percent.
Especially as shown in Figure 2 C, cleaning module has been equipped with 24 extraction column rotating disks, can realize the automatic switchover of 24 identical or different SPE posts.At work, first operator is placed in SPE post on rotating disk, is then walked SPE post is connected into purification stream by seal assembly 6 by system controlling software control rotating disk, completes the purified treatment of concentrate.The SPE post that this module is used is the Solid-Phase Extraction SPE decontaminating column of disposable comparative maturity, and commercialization for many years, therefore purifies detailed process and principle is not repeated.
As shown in Figure 2 D, concentrated constant volume module comprises concentrated cup, cold-trap, vacuum pump and infusion pump, completes the concentrated and constant volume of scavenging solution.Above-mentioned concentrated cup has been equipped with the rubber blanket bottle cap that can puncture, and can realize the importing of sample purification liquid under air-proof condition.In addition; the design of this module has adopted 24 fixing heating frames of concentrated cup; be used for placing 24 quantitatively concentrated cups and heating-up temperature is provided; each concentrated cup is connected by solenoid valve with vacuum pump; cold-trap between concentrated cup and vacuum pump is responsible for the cooling liquid of organic vapor and is reclaimed, and vacuum pump is shielded simultaneously.This module has been equipped with XYZ three-dimensional machinery arm simultaneously, on Z axis mechanical arm, has been equipped with puncture needle, can arrange the scavenging solution puncture containing target compound is imported in the quantitatively concentrated cup of setting by system.This module adopts the concentrated pattern that vacuumizes heating, can conveniently realize 1 to 24 successively or simultaneous quantitative concentrated.Concentrated cup bottom is equipped with liquid level detection device, can select two kinds of constant volumes of 1.5ml or 4ml, and constant volume pattern has the direct constant volume of infusion pump after laser infrared liquid level sensor constant volume or evaporate to dryness solution.Vacuumizing concentrated is technology well known to those skilled in the art, does not therefore do tired stating.
In sum, the invention provides a kind of can be automatically fast to food samples extract, concentrate, the intelligent system of purification and constant volume, once can unmanned complete the pre-treatment work of 24 complicated substrate samples.This system is mainly made up of extraction module, pre-concentration module, cleaning module and constant volume module four parts, completes instrument the order of 24 samples is processed continuously by tetrameric accurate cooperation.
Above-described embodiment is described the preferred embodiment of the present invention; not scope of the present invention is limited; design under the prerequisite of spirit not departing from the present invention; various distortion and improvement that the common engineering technical personnel in this area make technical scheme of the present invention, all should fall in the definite protection domain of claims of the present invention.
Claims (1)
1. the organic preprocessing system of food samples, is characterized in that: comprise the extraction module, pre-concentration module, cleaning module and the constant volume module that connect in turn; Extraction module comprises high-pressure pump (1), withstand voltage extraction and service sink (2), stream threeway, retaining valve, pressure unit (11), relief valve and stop valve; After described high-pressure pump (1), connect withstand voltage extraction and service sink (2) by stream threeway; Another path is again by stream threeway Connection Release valve and pressure unit (11) respectively; After pressure unit (11), connect retaining valve; Withstand voltage extraction and the rear stop valve that is connected of service sink (2);
Pre-concentration module comprises concentrated cup A (3), infusion pump A (4) and is located at the stop valve of concentrated cup A (3) lower end outlet, and emptying stop valve and nitrogen purge valve; Described concentrated cup A (3) bottom is provided with liquid level sensor (12);
Cleaning module comprises Solid-Phase Extraction SPE post (5) and seal assembly (6);
Constant volume module comprises concentrated cup B (8), cold-trap (9), vacuum pump (10) and infusion pump B (7).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210297569.XA CN102788722B (en) | 2012-08-20 | 2012-08-20 | Organic pretreatment system for food samples |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210297569.XA CN102788722B (en) | 2012-08-20 | 2012-08-20 | Organic pretreatment system for food samples |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102788722A CN102788722A (en) | 2012-11-21 |
| CN102788722B true CN102788722B (en) | 2014-10-22 |
Family
ID=47154189
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210297569.XA Expired - Fee Related CN102788722B (en) | 2012-08-20 | 2012-08-20 | Organic pretreatment system for food samples |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102788722B (en) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103063786A (en) * | 2012-12-27 | 2013-04-24 | 广东中烟工业有限责任公司 | A pretreatment device used for the analysis of tobacco-specific nitrosamines in cigarette smoke |
| WO2015074181A1 (en) * | 2013-11-19 | 2015-05-28 | 成都市产品质量监督检验院 | Nitrogen blowing apparatus and wet dissolving method using nitrogen blowing apparatus |
| CN104713753B (en) * | 2013-12-11 | 2019-03-29 | 北京六角体科技发展有限公司 | Sample control type preprocessing system |
| CN104316381B (en) * | 2014-11-05 | 2017-06-20 | 中国科学院生态环境研究中心 | The method of sample extraction, purification and concentration integrated device and sample pre-treatments |
| CN106198162A (en) * | 2016-06-24 | 2016-12-07 | 维科托（北京）科技有限公司 | Accelerate solvent extraction gel purification combined instrument and control method thereof |
| CN107817158A (en) * | 2017-09-01 | 2018-03-20 | 上海华之光谱仪器有限公司 | A kind of full-automatic rapid contractor and its extracting process for organic sample pre-treatment |
| CN110314412A (en) * | 2019-06-13 | 2019-10-11 | 南京康立瑞生物科技有限公司 | A kind of column chromatography for separation equipment for purifying |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101554602A (en) * | 2009-04-28 | 2009-10-14 | 储晓刚 | Full automatic liquid level tracing gas purging concentrator |
| CN101598739A (en) * | 2009-07-20 | 2009-12-09 | 中国检验检疫科学研究院 | A kind of full-automatic modular multi-sample intelligent processing system |
| WO2010087387A1 (en) * | 2009-01-29 | 2010-08-05 | 株式会社日立ハイテクノロジーズ | Device for pretreating sample and mass spectrometer equipped with same |
| CN101813582A (en) * | 2010-04-01 | 2010-08-25 | 北京市农林科学院 | Integrated pesticide residue detection pretreatment device and pretreatment method |
| CN102445552A (en) * | 2010-10-09 | 2012-05-09 | 武汉森济生物科技有限责任公司 | Automatic online multifunctional sample pretreatment equipment |
-
2012
- 2012-08-20 CN CN201210297569.XA patent/CN102788722B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2010087387A1 (en) * | 2009-01-29 | 2010-08-05 | 株式会社日立ハイテクノロジーズ | Device for pretreating sample and mass spectrometer equipped with same |
| CN101554602A (en) * | 2009-04-28 | 2009-10-14 | 储晓刚 | Full automatic liquid level tracing gas purging concentrator |
| CN101598739A (en) * | 2009-07-20 | 2009-12-09 | 中国检验检疫科学研究院 | A kind of full-automatic modular multi-sample intelligent processing system |
| CN101813582A (en) * | 2010-04-01 | 2010-08-25 | 北京市农林科学院 | Integrated pesticide residue detection pretreatment device and pretreatment method |
| CN102445552A (en) * | 2010-10-09 | 2012-05-09 | 武汉森济生物科技有限责任公司 | Automatic online multifunctional sample pretreatment equipment |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102788722A (en) | 2012-11-21 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102788722B (en) | Organic pretreatment system for food samples | |
| CN101509843B (en) | Sampling system for water filtrated by unattended shipborne multichannel film | |
| CN103235074B (en) | High performance liquid chromatography online analysis method and application thereof | |
| CN205176043U (en) | Water sample automatic acquisition and digestion instrument | |
| CN101813582A (en) | Integrated pesticide residue detection pretreatment device and pretreatment method | |
| CN101598739A (en) | A kind of full-automatic modular multi-sample intelligent processing system | |
| CN104007277B (en) | A kind of bio-toxicity automonitor and monitoring method | |
| CN102879257B (en) | A kind of full-automatic Accelerate solvent extraction-Solid-Phase Extraction combined instrument and extracting process thereof | |
| CN111443074A (en) | Automatic on-line pretreatment and Raman detection device and method thereof | |
| CN101762561B (en) | Method for on-line detecting integrity of ultrafiltration membrane by using ultraviolet monitoring method | |
| CN106198111A (en) | A kind of on-line sample acquisition and storage device | |
| CN202974733U (en) | Concentrating cup assembly for pretreatment of food samples | |
| ATE452666T1 (en) | METHOD AND DEVICE AS WELL AS CONNECTOR AND CONCENTRATE CONTAINER UNIT FOR PREPARING SOLUTIONS | |
| CN103969388B (en) | Perchlorate's on-line monitoring system | |
| CN202837076U (en) | Integral efficient solvent extracting and purifying device | |
| CN214150580U (en) | Liquid chromatographic column maintenance device | |
| CN106568624A (en) | A pathological specimen pretreatment device | |
| CN106872231B (en) | Soil hydrophobic fulvic acid component extraction purification device | |
| CN220877810U (en) | Cable type extraction and concentration integrated device | |
| CN207457159U (en) | More flux liquid-phase chromatographic column circle irrigation systems | |
| CN112179999A (en) | Sample extraction portion and residual solvent measurement device including the same | |
| CN208012920U (en) | A kind of substantially ponding sample preparation device | |
| CN205691554U (en) | A kind of pretreating device simultaneously carrying out acid and alkaline pigment detection | |
| KR20040059205A (en) | Apparatus for automatic preprocessing volatile organic compound | |
| CN101601967A (en) | A kind of four-channel full automatic gel permeation purification system for macromolecule |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20141022 Termination date: 20160820 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |