CN105301265B - On-line automaticization Magnetic solid phases micro-extraction desorbs detection means and its method - Google Patents
On-line automaticization Magnetic solid phases micro-extraction desorbs detection means and its method Download PDFInfo
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Abstract
The present invention relates to a kind of on-line automaticization Magnetic solid phases micro-extraction desorption detection means, including intelligence flowing sample injection device, sample loop, six-way valve, time-delay relay, magnet coil, quartz flow-cell, on-line detecting system, the intelligence flowing sample injection device controls four fluid pipelines by peristaltic pump P1, pump P2 under program, sample, adsorbent, water, strippant are conveyed respectively, and by switching six-way valve, specified liquid is delivered to ad-hoc location in special time, to realize extracting, desorb, wash carrying out in order for the steps such as pipeline.The magnet coil A and B is separately fixed at the upper and lower ends of quartz flow-cell, under time-delay relay control by magnetic adsorbent control in flow cell.The quartz flow-cell directly carries out on-line determination with ultraviolet specrophotometer combination.
Description
Technical field
The invention belongs to analytical chemistry instrument field, magnetic solid-phase extraction device is more particularly to automated, it is specially a kind of
On-line automaticization Magnetic solid phases micro-extraction-desorption-detection means and its method.
Background technology
Magnetic solid phases are extracted（Magnetic solid phase extraction, abbreviation MSPE）It is to separate 21 century
The revolutionary technology in enrichment field.MSPE is extracted as a kind of dispersed solid phase of adsorbent matrix using magnetic or magnetizable material
Take technology.Extracted with conventional solid（SPE）Filler is compared, and the specific surface area of nano particle is big, and diffusion length is short, it is only necessary to use
A small amount of adsorbent and shorter equilibration time can be achieved with the microextraction of low concentration, with extracting power and extraction very high
Take efficiency.At present, MSPE technologies are in cell separation, drug transport, enzyme immobilizatio, the absorption-separation of target organic, environment
High application prospect is all show in the numerous areas such as science, Food Science, genomics, protein science.
Because the conventional analysis of a large amount of samples often requires that quick, repeatable and data reliability, this has promoted automation to grasp
Make technology such as Flow Injection Analysis（FIA）, Sequential Injection Analysis（SIA）Etc. the development of correlation technique.The advantage of this kind of technology exists
Few in the solvent and amount of reagent of consumption, process time is short, low cost, and the rate of recovery and enrichment factor are higher.Therefore by MSPE
It is a kind of new technology for growing up in SPE field that technology is combined with Automated Ops technology.Lee etc.（Pei-Ling
Lee, Yuh-Chang Sun, Yong-Chien Ling, J. Anal. At. Spectrom., 2009, 24, 320–
327.）The article of MSPE application on site has been delivered first, and the detection architecture that automation MSPE devices and ICP-MS are constituted is used to
Determine content of beary metal.Chen etc.（Beibei Chen, Shujing Heng, Hanyong Peng, Bin Hu, Xu Yu,
Zhiling Zhang, Daiwen Pang, Xin Yue, Ying Zhu, Anal. At. Spectrom., 2010, 25,
1931–1938.）, Wang etc.（Yang Wang, Xiaoyu Luo, Jie Tang, Xiaoya Hu, Qin Xu, Chun
Yang, Anal. Chim. Acta., 2012, 713, 92–96.）, Giakisikli etc.（Georgia Giakisikli,
Aristidis N. Anthemidis, Talanta, 2013, 110, 229–235.）Will automation magnetic SPE dress
The measure for being applied to some metal ions in other field is put, has been pushed further into automating the hair of magnetic solid-phase extraction device
Exhibition.
All kinds of automation SPEs that the automation magnetic solid-phase extraction device for arriving referred to above occurs with the market
Device is compared, overcome that solid phase extraction method exists in itself the drawbacks of filling out the operations such as post, filtering or centrifugation, simplify and extracted
Journey, but apparatus above there is also some problems：First, magnetic material can only be controlled by the position of mobile micro-pipe external magnet
The state of material, malfunction, it is possible that with the nonsynchronous problem of other steps；Second, apparatus above and detecting system
Combination, being collection stripping liquid carries out on-line checking, and the method need to accurately judge the crucial opportunity of stripping liquid outflow, and essence in time
Stripping liquid is gathered accurately, and larger error easily occurs in this operation；3rd, after having processed a sample, need to supplement in time adsorbent or
The operations such as treatment micro-pipe, it is impossible to be carried out continuously sample analysis.Because apparatus above has these defects, therefore its scope of application is received
To considerable restraint, not yet occur using the instrument commodity of these principles so far.
The content of the invention
The present invention is to solve the above problems, there is provided a kind of on-line automaticization Magnetic solid phases micro-extraction-desorption-detection means
And its method.
The present invention adopts the following technical scheme that realization：
A kind of on-line automaticization Magnetic solid phases micro-extraction-desorption-detection means, including by intelligently flowing sample injection device control
The peristaltic pump P1 and peristaltic pump P2 of system.
The peristaltic pump P1 gathers the sample solution after dilution with magnetic absorption agent dispersing liquid by the way that caliber is different respectively
Tetrafluoroethene tube pump enters in sample loop, the sample loop by pipeline connect quartz flow-cell, the quartz flow-cell it is upper and lower
Motionless electromagnetic loop A and magnet coil B are distinguished in two ends, and the break-make of the magnet coil A and magnet coil B is by time-delay relay control
System；The quartz flow-cell carries out on-line determination with ultraviolet specrophotometer combination.
Conveyed respectively in the peristaltic pump P2 two polyfluortetraethylene pipes of water and strippant respectively with 2 mouthfuls of six-way valve and
3 mouthfuls connection, 1 mouthful of the six-way valve with the inlet communication of quartz flow-cell.
During work, sample is conveyed by the different polyfluortetraethylene pipe of two calibers of peristaltic pump P1 respectively with magnetic adsorbent
Mix in sample loop, and carry out auto extractive, object is attracted to magnetic material surface；When mixed liquor passes through quartz flow
When in pond, magnet coil A is powered, and magnetic material is attracted to quartz flow-cell upper end under the influence of a magnetic field, and waste liquid then by
Discharge；Then, under the conveying of peristaltic pump P2, water and strippant are respectively filled with pipeline, after six-way valve switching, the desorption in pipe
Agent is transferred in quartz flow-cell just under the conveying of water；Then, control quartz flow-cell upper and lower by time-delay relay
Magnet coil be alternately produced magnetic field, make the upper and lower fast vibration of adsorbent, be fully contacted with strippant, target molecule is to be solved
It is drawn in strippant；After desorption is complete, magnetic material is collected into quartz flow-cell upper end again under the influence of a magnetic field, this
When can carry out ultraviolet spectra on-line determination to the stripping liquid in quartz flow-cell；Finally, coil blackout, pumps into water cleaning pipeline,
Reclaim magnetic adsorbent, then the treatment for carrying out next sample.
Said apparatus invention purpose be：The device not only overcome automation solid-phase extraction device in fill out post, separate or
The troublesome operation processes such as centrifugation, and by time-delay relay make two magnet coils be alternately produced magnetic field to control magnetic absorption
Agent, it is easy to operate, it is easy to control to reach the purposes such as collection, desorption；The device is directly using quartz flow-cell as desorption
Pond, directly can carry out online spectral detection, without collecting stripping liquid after being parsed by quartz flow-cell, it is to avoid collection behaviour
The error that work is caused；The device controls two magnet coils to be alternately produced magnetic field by time-delay relay, and magnetic is controlled with this
Adsorbent, this avoids the loss of magnetic adsorbent, flexible and convenient operation；Before the next sample of device treatment, without changing
Or any part is processed, can constantly carry out sample treatment.
Compared with prior art, it is characteristic of the invention that：
1st, the device fills out the cumbersome operations such as post, separation or centrifugation in overcoming automation solid-phase extraction device completely
Journey, the characteristics of combine MSPE technologies, simplifies whole operation process, and operating efficiency is greatly improved.
2nd, whole device realizes intelligent, automation, serialization, under program, is automatically injected by peristaltic pump
Sample, adsorbent, water and parsing agent, by solenoid controlled magnetic adsorbent, with reach extraction, desorption, collection, detection,
The purposes such as washing pipeline.
3rd, this automation equipment directly carries out on-line checking with ultraviolet spectrometer combination, easy to operate, simple and quick, experiment
Error is greatly reduced.
4th, the present apparatus can carry out Treatment Analysis to low concentration bulk sample, and strippant consumption is few, and desorption volume can
μ L grades is reduced to, enrichment times are high, it is adaptable to set up highly sensitive analysis method.
5th, whole device simple structure, every time after the completion of extraction, desorption, detection, waste liquid and adsorbent etc. can be automatically drained out,
Any part need not be dismantled to be changed or other treatment, and one sample of Treatment Analysis only takes 8min, high working efficiency can
The analysis for being carried out continuously batch samples is determined.
6th, detection is analyzed using automation equipment, reduces the error that manual operation brings, measurement result is accurate, essence
Density is high, favorable reproducibility.
7th, the repeatable recycling of magnetic adsorbent dispersant used is extracted, cost is relatively low, and selection is flexible.
During completion is of the invention, the property indices to the device are tested repeatedly, with good
Stability.Its reappearance RSD≤1.8%.
Reasonable in design, simple structure of the invention, the intelligent automation device continuously can carry out low dense to multigroup sample solution
Degree large volume extraction, small size desorption, enrichment times are high, and sensitivity is high, and convenient operation, are greatly saved manpower and materials,
Operating efficiency is improve, automation, intellectuality, the serialization of whole operation flow is realized.
Brief description of the drawings
Fig. 1 represents connection diagram of the invention.
In figure, 1- sample loops, 2- quartz flow-cells, 3- time-delay relays, 4- ultraviolet specrophotometers, 5- six-way valves.
Specific embodiment
The present invention is further described below by example combination accompanying drawing, but range of application of the invention and is not only limited
In this.
A kind of on-line automaticization Magnetic solid phases micro-extraction-desorption-detection means, including intelligence flowing sample injection device, sample
Product ring, six-way valve, time-delay relay, magnet coil, quartz flow-cell, on-line detecting system.Intelligence flowing sample injection device exists
Four fluid pipelines of peristaltic pump P1 and peristaltic pump P2 are controlled under programme-control, sample, adsorbent, water, strippant are conveyed respectively,
And by switching six-way valve, specified liquid is delivered to ad-hoc location in special time, to realize extracting, desorb, wash pipeline
Etc. carrying out in order for step.Magnet coil is fixed on the upper/lower terminal outside quartz flow-cell, by magnetic under time-delay relay control
Property adsorbent control in quartz flow-cell upper and lower side.Quartz flow-cell is directly surveyed online with ultraviolet specrophotometer combination
It is fixed.
Concrete structure is as follows：
As shown in figure 1, on-line automaticization Magnetic solid phases micro-extraction-desorption-detection means includes being injected into by intelligence flowing
The peristaltic pump P1 and peristaltic pump P2 of sample device control.
As shown in figure 1, the sample solution after dilution and magnetic absorption agent dispersing liquid are passed through pipe by the peristaltic pump P1 respectively
The different polyfluortetraethylene pipe in footpath is pumped into sample loop 1, and the sample loop 1 connects quartz flow-cell 2, the quartz by pipeline
Upper and lower ends difference Motionless electromagnetic loop A and the magnet coil B of flow cell 2, the break-make of the magnet coil A and magnet coil B
Controlled by time-delay relay 3；The quartz flow-cell 2 carries out on-line determination with the combination of ultraviolet specrophotometer 4.
As shown in figure 1, two polyfluortetraethylene pipes of water and strippant are conveyed in the peristaltic pump P2 respectively respectively with six
2 mouthfuls of port valve 5 and 3 mouthfuls connection, 1 mouthful of the six-way valve 5 with the inlet communication of quartz flow-cell 2.
The sample solution after dilution and magnetic absorption agent dispersing liquid are led to simultaneously respectively by intelligently flowing sample injection device
Cross two different polyfluortetraethylene pipes of caliber and pump into sample loop and be well mixed, and carry out auto extractive；By magnet coil
Magnetic adsorbent is collected into quartz flow-cell, waste liquid is discharged；Then to stripping liquid is pumped into flow cell, by time delay relay
Device controls two magnet coils to be alternately produced magnetic field, and magnetic adsorbent vertical tremor in flow cell makes analyte desorption complete.
Magnetic adsorbent is collected to quartz flow-cell upper end, stripping liquid, record data are determined by ultraviolet specrophotometer；Finally,
Discharge waste liquid, reclaims magnetic adsorbent, and cleaning device pipeline prepares next group of sample for the treatment of.
On-line automaticization Magnetic solid phases micro-extraction is carried out below with said apparatus quickly determine light blue in presetting cocktail
The method of content, it is comprised the following steps that：
1st, on-line automaticization Magnetic solid phases micro-extraction-desorption-detection means parameter setting is as follows：
2nd, sample is processed：The presetting cocktail of certain brand of a certain amount of local supermarket's purchase is taken, 10mL is settled to.
3rd, the extraction of automation magnetic and desorption：It is pre- by intelligence flowing sample injection device 10mL is diluted respectively simultaneously after
Adjust cocktail sample to be pumped into sample loop by two different polyfluortetraethylene pipes of caliber with 2mL magnetic absorptions agent dispersing liquid to mix
Close uniform, and carry out auto extractive, magnetic adsorbent is collected into the quartz flow-cell of 0.3mL by magnet coil, discharge
Waste liquid；Then to stripping liquid is pumped into flow cell, control magnet coil A and B to be alternately produced magnetic field by time-delay relay, make magnetic
Property adsorbent vertical tremor 30s in flow cell, makes analyte desorption complete.
4th, online spectral detection：After the completion of desorption, magnetic adsorbent is collected to quartz flow-cell upper end, by ultraviolet point
Light photometric determination stripping liquid, record data is calculated the content of light blue in presetting cocktail sample.
The content that contained light blue in presetting cocktail sample is surveyed in this experiment is 3.28mg/kg.
It should be noted last that, the above embodiments are merely illustrative of the technical solutions of the present invention and it is unrestricted, although ginseng
It has been described in detail according to the embodiment of the present invention, it will be understood by those within the art that, to technical scheme
Modify or equivalent, without departure from the spirit and scope of technical scheme, it all should cover of the invention
In claims.
Claims (1)
1. a kind of on-line automaticization Magnetic solid phases micro-extraction-desorption-detection method, it is characterised in that：
On-line automaticization Magnetic solid phases micro-extraction-desorption-detection means includes the wriggling by intelligently flowing the control of sample injection device
Pump P1 and peristaltic pump P2；
Sample solution after dilution is passed through the different polytetrafluoro of caliber with magnetic absorption agent dispersing liquid by the peristaltic pump P1 respectively
Ethylene tube pumps into sample loop（1）It is interior, the sample loop（1）Quartz flow-cell is connected by pipeline（2）, the quartz flow-cell
（2）Upper and lower ends difference Motionless electromagnetic loop A and magnet coil B, the break-make of the magnet coil A and magnet coil B is by prolonging
When relay（3）Control；The quartz flow-cell（2）With ultraviolet specrophotometer（4）Combination carries out on-line determination；
Conveyed respectively in the peristaltic pump P2 two polyfluortetraethylene pipes of water and strippant respectively with six-way valve（5）2 mouthfuls and 3
Mouth connection, the six-way valve（5）1 mouthful and quartz flow-cell（2）Inlet communication；
Specific method comprises the following steps：
（1）, intelligence flowing sample injection device control peristaltic pump P1 simultaneously disperses the sample solution after dilution and magnetic adsorbent
Liquid pumps into sample loop by two different polyfluortetraethylene pipes of caliber（1）It is interior well mixed, and carry out auto extractive, object
It is attracted to magnetic material surface；
（2）, to positioned at quartz flow-cell（2）The magnet coil A or magnet coil B of upper end or lower end are powered, by magnetic absorption
Agent is collected into quartz flow-cell（2）Upper end or lower end in, discharge waste liquid；
（3）, under intelligence flowing sample injection device control peristaltic pump P2 conveyings, water and strippant respectively filled with pipeline, by switching
After six-way valve, the strippant in pipe is transferred to quartz flow-cell just under the conveying of water（2）It is interior；
（4）, by time-delay relay（3）Control quartz flow-cell（2）Upper and lower magnet coil A and magnet coil B is alternately produced
Magnetic field, makes the upper and lower fast vibration of adsorbent, is fully contacted with strippant, and target molecule is to be desorbed into strippant；
（5）, when desorption completely after, magnetic material is collected into quartz flow-cell in the presence of magnet coil A（2）Interior upper end,
Now to quartz flow-cell（2）Interior stripping liquid utilizes ultraviolet specrophotometer（4）Carry out ultraviolet spectra on-line determination；
（6）, last, magnet coil power-off, pump into water cleaning pipeline, reclaim magnetic adsorbent, then the treatment for carrying out next sample.
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| CN107402154A (en) * | 2017-09-18 | 2017-11-28 | 中国地质科学院郑州矿产综合利用研究所 | Automatic change magnetism solid phase extraction device |
| CN109225165B (en) * | 2018-08-27 | 2021-05-11 | 西北大学 | Preparation method and application of silicｃA @ P-A-betｃA-CD/NIPAM adsorption medium |
| CN110470758B (en) * | 2019-08-14 | 2020-09-08 | 厦门大学 | Device and analysis method for on-line detection of sulfonylurea pesticide residues in environmental water sample |
| CN112834298B (en) * | 2020-12-30 | 2022-01-28 | 山西大学 | Anti-pollution sample processing system |
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