CN208420807U - A kind of pump of bivalve three highly effective liquid phase chromatographic system - Google Patents
A kind of pump of bivalve three highly effective liquid phase chromatographic system Download PDFInfo
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- CN208420807U CN208420807U CN201821252005.3U CN201821252005U CN208420807U CN 208420807 U CN208420807 U CN 208420807U CN 201821252005 U CN201821252005 U CN 201821252005U CN 208420807 U CN208420807 U CN 208420807U
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Abstract
The utility model relates to a kind of bivalves three to pump highly effective liquid phase chromatographic system, including Solid Phase Extraction sampling pump, external six-way valve, solid-phase extraction column, One Dimension Analysis column, variable-wavelenght detector, two-dimentional trapping column, two-dimension analysis column, six-way valve in case, Solid Phase Extraction sampling pump is connect with autosampler, autosampler, waste collecting device, One Dimension Analysis pump respectively with No. 4 mouths of external six-way valve, No. 6 mouths, No. 8 mouth connections, solid-phase extraction column is connect with No. 5 mouths of external six-way valve and No. 7 mouths, One Dimension Analysis column is connect with No. 14 mouths of six-way valve in No. 9 mouths of external six-way valve and case, variable-wavelenght detector, two-dimension analysis pump respectively with No. 15 mouths of six-way valve in case, No. 17 mouth connections, No. 16 mouths of six-way valve in two-dimentional trapping column and case, No. 19 mouth connections, No. 18 mouths of six-way valve and two poles in two-dimension analysis column and case The connection of pipe array detector；The utility model simplifies sample pre-treatments operating procedure, improves the analysis efficiency of sample.
Description
[technical field]
The utility model relates to high-efficient liquid phase chromatogram technology field, specifically a kind of bivalve three pumps high performance liquid chromatography
System.
[background technique]
Since the use of chromatography in 1903, various chromatographic techniques come into being, and wherein high performance liquid chromatography is due to analysis
The advantages that speed is fast, separative efficiency is high, detection sensitivity is high, detection automates, is applied widely, becomes the most commonly used separation
And detection means, it is all widely used in fields such as materia medica, Food Science, environmental monitorings.Since the 21th century, chromatography skill
The development of art is gradually mature, and basic innovation achievement is extremely limited, but technical progress is carrying out always, especially
Action oriented research relevant to industry is still very active.
Nutrient health research institute of China Oil and Food Import and Export Corporation Xie Yunfeng in 2014 etc. reports on-line solid phase extraction-high performance liquid chromatography combination and surveys
Determine vitamin A in animal-derived food, the method for E, this method is passed through using double gradient liquid chromatography system combination column switching techniques
One valve two pump and the flow path switching setting between solid-phase extraction column and analytical column realize on-line solid phase extraction and high-efficient liquid phase color
The combination of spectrum.Though the method realizes in-line purification, in vitamin A, the analysis of D, E, the problem of due to method sensitivity, only
Suitable for analyzing vitamin A, E.Soon, match is silent flies to have issued online two-dimensional columns switching method while measuring vitamin A in feed, D,
The solution of E, this method using online two-dimensional columns switching combine high performance liquid chromatography, by two valves two pump two and analytical column it
Between flow path switching setting realize vitamin A, D, E single injected sampling while, is detected.But since method pre-treatment still needs to be saponified
Extraction concentration and etc., pretreatment process very complicated, time-consuming consumption manpower largely effects on the analysis efficiency of sample.
[utility model content]
The purpose of this utility model seeks to solve above-mentioned deficiency and provide a kind of pump of bivalve three high-efficient liquid phase color pedigree
System, the system can be applied to vitamin A in milk powder, and the content measuring of D, E can greatly simplify sample pre-treatments operating procedure,
Manpower and reagent cost are saved, the analysis efficiency of sample is significantly improved.
Design a kind of bivalve three to achieve the above object and pump highly effective liquid phase chromatographic system, including Solid Phase Extraction sampling pump 1, from
Dynamic sample injector 2, external six-way valve 3, waste collecting device 10, solid-phase extraction column 11, One Dimension Analysis pump 12, One Dimension Analysis column 13,
Variable-wavelenght detector 20, two-dimension analysis pump 21, two-dimentional trapping column 22, two-dimension analysis column 23, diode array detector 24, case
Interior six-way valve 25, the external six-way valve 3 are equipped with external first valve port 4, external second valve port 5, external third valve port 6, outer
Set the 4th valve port 7, external 5th valve port 8, external 6th valve port 9, in the case six-way valve 25 be equipped with case in the first valve port 14,
Second valve port 15 in case, third valve port 16 in case, the 4th valve port 17 in case, the 5th valve port 18 in case, the 6th valve port 19 in case, institute
It states Solid Phase Extraction sampling pump 1 to connect with autosampler 2, external the of 2 other end of autosampler and external six-way valve 3
One valve port 4 connection, 11 both ends of solid-phase extraction column respectively with external second valve port 5 of external six-way valve 3 and external 4th valve
Mouthfuls 7 connect, and the waste collecting device 10 connect with the external third valve port 6 of external six-way valve 3, the One Dimension Analysis pump 12 and
External 5th valve port 8 of external six-way valve 3 connects, external 6th valve of described 13 one end of One Dimension Analysis column and external six-way valve 3
Mouthfuls 9 connect, 13 other end of One Dimension Analysis column with first send out valve port 14 in the case of six-way valve 25 in case and connect, the variable wave
Long detector 20 with second valve port 15 is connect in the case of six-way valve 25 in case, two dimension trapping column 22 both ends are respectively in case six
6th valve port 19 connection in third valve port 16 and case in the case of port valve 25, the case of the two-dimension analysis pump 21 and six-way valve 25 in case
The connection of interior 4th valve port 17, described 23 one end of two-dimension analysis column with the 5th valve port 18 is connect in the case of six-way valve 25 in case, it is described
23 other end of two-dimension analysis column is connect with diode array detector 24.
It further, further include control system, the control system is 2.2 chromatography data system of OPENLAB CDS.
Further, external second valve port 5, external first valve port 4, external third valve port 6, external 4th valve port 7,
External 5th valve port 8, external 6th valve port 9 along external six-way valve 3 circumferentially, the first valve port 14 in the case, second in case
Third valve port 16 in valve port 15, case, the 4th valve port 17 in case, the 5th valve port 18 in case, the 6th valve port 19 is six logical along case in case
Valve 25 is circumferentially.
The utility model compared with the existing technology, has the advantages that
(1) the utility model establishes a kind of pumping equipped with bivalve three, it can be achieved that online solid phase for a variety of separating mechanisms of combination
The highly effective liquid phase chromatographic system of extracting and purifying and analysis, and it is applied to vitamin A in milk powder, the content measuring of D, E, once
Sample introduction detects simultaneously, simplifies operating procedure, greatly shortens the time of pre-treatment, saves manpower and reagent cost, and realization exists automatically
Line purification detection, improves sensitivity, guarantees the accuracy and reproducibility of test result, prevent vitamin enrichment dosage not from source
Standard is adversely affected to consumer health's bring.
(2) the utility model is the highly effective liquid phase chromatographic system that four root chromatogram columns of connection are pumped equipped with bivalve three, passes through solid phase
Extraction and highly effective liquid phase chromatographic system on-line joining process realize the purification and two dimension of sample solution in combination with column switching technique
The automatic connection of chromatography；Solid-phase extraction column in-line purification analytical solution, one-dimensional chromatography partial target object.Two way chromatograms
Analysis part object；Meanwhile trapping column has been used in Two way chromatograms for the first time, it efficiently solves since object is in Two way chromatograms
Due to caused by diffusion phenomena the problem of chromatographic peak wide sensitivity decrease during distribution behavior.
(3) it after object is enriched in decontaminating column and trapping column in the utility model, is all made of opposite with purification process flow path
The mode of direction elution, object is transferred in analytical column, the chromatographic peak of acquisition, peak width is moderate, and symmetry is good.
(4) chromatographic column filler used in the utility model is the substance of resistance to highly basic.
(5) the utility model is successfully applied in vitamin A in milk powder, directly fixed by saponification liquor while D, E in measurement
Upper machine analysis after appearance greatly simplifies sample pre-treatments behaviour the step of cleverly avoiding organic solvent phase inversion, concentration, redissolve
Make step, significantly improves the analysis efficiency of sample.Simultaneously as pretreatment process simplifies, vitamin A is reduced, D, E are being analyzed
The risk of oxidative degradation in the process, it is ensured that the accuracy and reproducibility of test result.
[Detailed description of the invention]
Analytical solution flow path schematic diagram when Fig. 1 is the utility model SPE loading；
Fig. 2 is the utility model SPE elution, analytical solution flow path schematic diagram when object is transferred to one-dimensional chromatographic column；
Fig. 3 is the utility model SPE cleaning, and analytical solution flow path is illustrated when partial target object is eluted from one-dimensional chromatographic column
Figure；
Fig. 4 is the utility model SPE cleaning, analytical solution stream when partial target object is transferred to trapping column from one-dimensional chromatographic column
Road schematic diagram；
Fig. 5 be the utility model SPE balance, partial target object from trapping column transfer be two-dimension analysis column when analytical solution stream
Road schematic diagram；
In figure: 1, Solid Phase Extraction sampling pump 2, autosampler 3, external six-way valve 4, external first valve port 5, external
Second valve port 6, external third valve port 7, external 4th valve port 8, external 5th valve port 9, external 6th valve port 10, waste liquid
Collection device 11, solid-phase extraction column 12, One Dimension Analysis pump 13, One Dimension Analysis column 14, the first valve port 15 in case, the in case
Third valve port 17 in two valve ports 16, case, the 4th valve port 18 in case, the 5th valve port 19 in case, the 6th valve port 20 in case, can
Become wavelength detecting 21, two-dimension analysis pump 22, two-dimentional trapping column 23, two-dimension analysis column 24, diode array detector
25, six-way valve in case.
[specific embodiment]
The pump of bivalve three of being furnished with that the utility model provides a kind of a variety of separating mechanisms of combination connects four root chromatogram columns, can be real
Present line Solid phase extraction and the bivalve three of analysis pump highly effective liquid phase chromatographic system, including Solid Phase Extraction sampling pump 1, automatically into
Sample device 2, waste collecting device 10, solid-phase extraction column 11, One Dimension Analysis pump 12, One Dimension Analysis column 13, can be changed external six-way valve 3
Wavelength detecting 20, two-dimension analysis pump 21, two-dimentional trapping column 22, two-dimension analysis column 23, diode array detector 24, six in case
Port valve 25, external six-way valve 3 are equipped with external first valve port 4, external second valve port 5, external third valve port 6, external 4th valve
Mouthful 7, external 5th valve port 8, external 6th valve port 9, six-way valve 25 is equipped with the first valve port 14 in case, the second valve port in case in case
15, third valve port 16 in case, the 4th valve port 17 in case, the 5th valve port 18 in case, the 6th valve port 19 in case；Solid Phase Extraction sampling pump
1 connect with autosampler 2, absorption and sample introduction for realizing sample analysis solution；2 other end of autosampler and external six
External first valve port 4 of port valve 3 connects；11 both ends of solid-phase extraction column respectively with external second valve port 5 of external six-way valve 3 and outer
The connection of the 4th valve port 7 is set, positive flow path is for realizing the primary purification of sample analysis solution, and reversed flow path is for realizing enrichment
The elution sample introduction of analyte；Waste collecting device 10 is connect with the external third valve port 6 of external six-way valve 3, for collecting elution
Liquid；One Dimension Analysis pump 12 and external 5th valve port 8 of external six-way valve 3 connect, and flow the One Dimension Analysis column 13 that balances each other for transporting
The object of solid-phase extraction column 11 is enriched in reversed elution；13 one end of One Dimension Analysis column and the external 6th of external six-way valve 3
Valve port 9 connects, 13 other end of One Dimension Analysis column with first valve port 14 is connect in the case of six-way valve 25 in case, for analysis portion subhead
Mark object；Variable-wavelenght detector 20 with second valve port 15 is connect in the case of six-way valve 25 in case, for detecting object；Two dimension is caught
Obtain 22 both ends of column respectively with the 6th valve port 19 is connect in third valve port 16 and case in the case of six-way valve 25 in case, positive flow path is used
In realize enrichment of analyte elution sample introduction, reversed flow path for realizing sample analysis solution double purification；Two-dimension analysis pump
21 with the 4th valve port 17 is connect in the case of six-way valve 25 in case, balance each other two-dimension analysis column 23 and positive elution for transporting flowing
It is enriched in the object of two-dimentional trapping column 22；The 5th valve port 18 connects in the case of six-way valve 25 in 23 one end of two-dimension analysis column and case
It connects, 23 other end of two-dimension analysis column is connect with diode array detector 24, for detecting object.
In the utility model, external second valve port 5, external first valve port 4, external third valve port 6, external 4th valve port 7,
External 5th valve port 8, external 6th valve port 9 along external six-way valve 3 circumferentially, the first valve port 14 in case, the second valve port in case
15, third valve port 16 in case, the 4th valve port 17 in case, the 5th valve port 18 in case, the 6th six-way valve 25 along case of valve port 19 in case
Circumferentially；Further include control system, control system is 2.2 chromatography data system of OPENLAB CDS, using control platform and
Connection and communication are established between power supply system and each device, and personnel's operation is substituted by control test macro, it is automatic using this
Change testing process to be tested.
When solid-phase extraction column is in loading state, One Dimension Analysis column, two-dimentional trapping column and two-dimension analysis column are in balance
State, external six-way valve flow path setting are as follows: 2 → 4 → 5 → 7 → 6 → 10；12→8→9→13；Six-way valve flow path is arranged in case
Are as follows: 13 → 14 → 15 → 20；21→17→16→19→18→23.
When solid-phase extraction column is in elution state, object is transferred to one-dimensional chromatographic column, two-dimentional trapping column and two dimension point
Analysis column is in equilibrium state, external six-way valve flow path setting are as follows: 12 → 8 → 7 → 5 → 9 → 13；2→4→6→10；Six is logical in case
Valve flow path setting are as follows: 13 → 14 → 15 → 20；21→17→16→19→18→23.
When solid-phase extraction column, which is in, washes down state, object is eluted from one-dimensional chromatographic column, two-dimentional trapping column and two dimension point
Analysis column is in equilibrium state, external six-way valve flow path setting are as follows: 2 → 4 → 5 → 7 → 6 → 10；12→8→9→13；Six is logical in case
Valve flow path setting are as follows: 13 → 14 → 15 → 20；21→17→16→19→18→23.
When solid-phase extraction column, which is in, washes down state, partial target object is transferred to two-dimentional trapping column from one-dimensional chromatographic column, and two
Dimension analytical column is in equilibrium state, external six-way valve flow path setting are as follows: 2 → 4 → 5 → 7 → 6 → 10；12→8→9→13；In case
Six-way valve flow path setting are as follows: 21 → 17 → 18 → 23；13→14→19→16→15→20.
When solid-phase extraction column is in equilibrium state, partial target object is transferred to two-dimension analysis column from two-dimentional trapping column, and one
Dimension analytical column is in equilibrium state, external six-way valve flow path setting are as follows: 2 → 4 → 5 → 7 → 6 → 10；12→8→9→13；In case
Six-way valve flow path setting are as follows: 13 → 14 → 15 → 20；21→17→16→19→18→23.
The utility model can be successfully applied to vitamin A in milk powder, and the test of D, E pass through Solid Phase Extraction and efficient liquid phase
Chromatographic system on-line joining process realizes the automatic connection of purification and the Two way chromatograms analysis of sample solution.One-dimensional chromatography portion
Partial objectives for object, Two way chromatograms analysis part object.Used trapping column for the first time in Two way chromatograms simultaneously, efficiently solve due to
Object during chromatography distribution behavior due to diffusion phenomena caused by chromatographic peak wide sensitivity decrease the problem of.
Vitamin A in the highly effective liquid phase chromatographic system measurement milk powder described in the utility model pumped equipped with bivalve three, D, E's
Method, comprising the following steps:
1) sample treatment: powdered milk sample is mixed, and weighs appropriate, addition water, dehydrated alcohol, ascorbic acid, BHT and KOH
Aqueous solution, heating saponification, cooling constant volume after the completion of saponification.
2) using the high performance liquid chromatograph determination step 1 for being furnished with bivalve three pump system) whether contain in resulting solution
Vitamin A, D, E: if one-dimensional liquid chromatography results show that sample is doubtful containing vitamin A, when E, then comparative sample and vitamin
The retention time of A, E standard substance, whether to contain vitamin A, E in confirmatory sample；If two-dimensional liquid chromatography shows that sample is doubted
When like containing vitamin D, then whether the retention time of comparative sample and vitamin D standard substance, tieed up with containing in confirmatory sample
Raw element D.
If 3) contain vitamin A in confirmatory sample, D, E then calculate vitamin A in sample, the content of D, E by formula.
The utility model is simultaneously not limited to the embodiments described above, and other any spirit without departing from the utility model are real
Made changes, modifications, substitutions, combinations, simplifications under matter and principle, should be equivalent substitute mode, be included in practical
Within novel protection scope.
Claims (3)
1. a kind of bivalve three pumps highly effective liquid phase chromatographic system, it is characterised in that: including Solid Phase Extraction sampling pump (1), automatic sampling
Device (2), external six-way valve (3), waste collecting device (10), solid-phase extraction column (11), One Dimension Analysis pump (12), One Dimension Analysis column
(13), variable-wavelenght detector (20), two-dimension analysis pump (21), two-dimentional trapping column (22), two-dimension analysis column (23), diode battle array
Six-way valve (25) in column detector (24), case, the external six-way valve (3) are equipped with external first valve port (4), external second valve
Mouth (5), external third valve port (6), external 4th valve port (7), external 5th valve port (8), external 6th valve port (9), the case
Interior six-way valve (25) is equipped with the first valve port (14) in case, the second valve port (15) in case, third valve port (16) in case, the 4th in case
5th valve port (18) in valve port (17), case, the 6th valve port (19), the Solid Phase Extraction sampling pump (1) and autosampler in case
(2) it connects, autosampler (2) other end is connect with external first valve port (4) of external six-way valve (3), the solid phase
Extraction column (11) both ends are connect with external second valve port (5) of external six-way valve (3) and external 4th valve port (7) respectively, described
Waste collecting device (10) is connect with the external third valve port (6) of external six-way valve (3), One Dimension Analysis pump (12) with it is external
External 5th valve port (8) of six-way valve (3) connects, and external the of described One Dimension Analysis column (13) one end and external six-way valve (3)
Six valve ports (9) connection, One Dimension Analysis column (13) other end are connect with the first valve port (14) in the case of six-way valve in case (25),
The variable-wavelenght detector (20) connect with the second valve port (15) in the case of six-way valve in case (25), the two dimension trapping column
(22) both ends are connect with the 6th valve port (19) in third valve port (16) in the case of six-way valve in case (25) and case respectively, the two dimension
Analysis pump (21) is connect with the 4th valve port (17) in the case of six-way valve in case (25), in described two-dimension analysis column (23) one end and case
The 5th valve port (18) connects in the case of six-way valve (25), two-dimension analysis column (23) other end and diode array detector
(24) it connects.
2. the system as claimed in claim 1, it is characterised in that: further include control system, the control system is OPENLAB
2.2 chromatography data system of CDS.
3. the system as claimed in claim 1, it is characterised in that: external second valve port (5), external first valve port (4), outer
Third valve port (6), external 4th valve port (7), external 5th valve port (8), external 6th valve port (9) are set along external six-way valve (3)
Circumferentially, the first valve port (14) in the case, the second valve port (15) in case, third valve port (16) in case, the 4th valve port in case
(17), the 5th valve port (18) in case, six-way valve (25) is circumferentially along case for the 6th valve port (19) in case.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201821252005.3U CN208420807U (en) | 2018-08-06 | 2018-08-06 | A kind of pump of bivalve three highly effective liquid phase chromatographic system |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201821252005.3U CN208420807U (en) | 2018-08-06 | 2018-08-06 | A kind of pump of bivalve three highly effective liquid phase chromatographic system |
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| Publication Number | Publication Date |
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| CN208420807U true CN208420807U (en) | 2019-01-22 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201821252005.3U Active CN208420807U (en) | 2018-08-06 | 2018-08-06 | A kind of pump of bivalve three highly effective liquid phase chromatographic system |
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| CN (1) | CN208420807U (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108760941A (en) * | 2018-08-06 | 2018-11-06 | 通标标准技术服务(上海)有限公司 | A kind of pump of bivalve three highly effective liquid phase chromatographic system |
| CN115219603A (en) * | 2021-04-15 | 2022-10-21 | 仙乐健康科技股份有限公司 | Method for simultaneously determining vitamins A, D and E in sample |
-
2018
- 2018-08-06 CN CN201821252005.3U patent/CN208420807U/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108760941A (en) * | 2018-08-06 | 2018-11-06 | 通标标准技术服务(上海)有限公司 | A kind of pump of bivalve three highly effective liquid phase chromatographic system |
| CN115219603A (en) * | 2021-04-15 | 2022-10-21 | 仙乐健康科技股份有限公司 | Method for simultaneously determining vitamins A, D and E in sample |
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