CN108760941A - 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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- CN108760941A CN108760941A CN201810882195.5A CN201810882195A CN108760941A CN 108760941 A CN108760941 A CN 108760941A CN 201810882195 A CN201810882195 A CN 201810882195A CN 108760941 A CN108760941 A CN 108760941A
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- 239000007791 liquid phase Substances 0.000 title claims abstract description 17
- 238000004458 analytical method Methods 0.000 claims abstract description 89
- 238000002414 normal-phase solid-phase extraction Methods 0.000 claims abstract description 43
- 238000005070 sampling Methods 0.000 claims abstract description 12
- 239000002699 waste material Substances 0.000 claims abstract description 8
- FPIPGXGPPPQFEQ-UHFFFAOYSA-N 13-cis retinol Natural products OCC=C(C)C=CC=C(C)C=CC1=C(C)CCCC1(C)C FPIPGXGPPPQFEQ-UHFFFAOYSA-N 0.000 claims description 26
- FPIPGXGPPPQFEQ-BOOMUCAASA-N Vitamin A Natural products OC/C=C(/C)\C=C\C=C(\C)/C=C/C1=C(C)CCCC1(C)C FPIPGXGPPPQFEQ-BOOMUCAASA-N 0.000 claims description 26
- FPIPGXGPPPQFEQ-OVSJKPMPSA-N all-trans-retinol Chemical compound OC\C=C(/C)\C=C\C=C(/C)\C=C\C1=C(C)CCCC1(C)C FPIPGXGPPPQFEQ-OVSJKPMPSA-N 0.000 claims description 26
- 235000019155 vitamin A Nutrition 0.000 claims description 26
- 239000011719 vitamin A Substances 0.000 claims description 26
- 229940045997 vitamin a Drugs 0.000 claims description 26
- 238000000034 method Methods 0.000 claims description 19
- 238000010828 elution Methods 0.000 claims description 15
- 238000000746 purification Methods 0.000 claims description 12
- 238000004587 chromatography analysis Methods 0.000 claims description 9
- 238000007127 saponification reaction Methods 0.000 claims description 8
- 229930003316 Vitamin D Natural products 0.000 claims description 7
- QYSXJUFSXHHAJI-XFEUOLMDSA-N Vitamin D3 Natural products C1(/[C@@H]2CC[C@@H]([C@]2(CCC1)C)[C@H](C)CCCC(C)C)=C/C=C1\C[C@@H](O)CCC1=C QYSXJUFSXHHAJI-XFEUOLMDSA-N 0.000 claims description 7
- 235000013336 milk Nutrition 0.000 claims description 7
- 239000008267 milk Substances 0.000 claims description 7
- 210000004080 milk Anatomy 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 7
- 235000019166 vitamin D Nutrition 0.000 claims description 7
- 239000011710 vitamin D Substances 0.000 claims description 7
- 150000003710 vitamin D derivatives Chemical class 0.000 claims description 7
- 229940046008 vitamin d Drugs 0.000 claims description 7
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 6
- 239000012491 analyte Substances 0.000 claims description 6
- 230000000052 comparative effect Effects 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 230000014759 maintenance of location Effects 0.000 claims description 6
- 238000004811 liquid chromatography Methods 0.000 claims description 4
- 238000011068 loading method Methods 0.000 claims description 4
- 229940088594 vitamin Drugs 0.000 claims description 4
- 229930003231 vitamin Natural products 0.000 claims description 4
- 235000013343 vitamin Nutrition 0.000 claims description 4
- 239000011782 vitamin Substances 0.000 claims description 4
- 150000003722 vitamin derivatives Chemical class 0.000 claims description 4
- 238000004780 2D liquid chromatography Methods 0.000 claims description 3
- NLZUEZXRPGMBCV-UHFFFAOYSA-N Butylhydroxytoluene Chemical compound CC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 NLZUEZXRPGMBCV-UHFFFAOYSA-N 0.000 claims description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 3
- 238000010521 absorption reaction Methods 0.000 claims description 3
- 235000010323 ascorbic acid Nutrition 0.000 claims description 3
- 229960005070 ascorbic acid Drugs 0.000 claims description 3
- 239000011668 ascorbic acid Substances 0.000 claims description 3
- 235000010354 butylated hydroxytoluene Nutrition 0.000 claims description 3
- 239000003480 eluent Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 235000011118 potassium hydroxide Nutrition 0.000 claims description 3
- 235000008476 powdered milk Nutrition 0.000 claims description 3
- 238000011282 treatment Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims 1
- 238000002203 pretreatment Methods 0.000 abstract description 5
- 238000011017 operating method Methods 0.000 abstract description 3
- 239000000523 sample Substances 0.000 description 37
- 239000000243 solution Substances 0.000 description 15
- 230000008569 process Effects 0.000 description 8
- 238000012360 testing method Methods 0.000 description 7
- 230000035945 sensitivity Effects 0.000 description 5
- 238000001514 detection method Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 235000013305 food Nutrition 0.000 description 3
- 238000004128 high performance liquid chromatography Methods 0.000 description 3
- 230000009471 action Effects 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000012488 sample solution Substances 0.000 description 2
- 230000002411 adverse Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000686 essence Substances 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 239000002398 materia medica Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000010525 oxidative degradation reaction Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/60—Construction of the column
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/64—Electrical detectors
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/027—Liquid chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Treatment Of Liquids With Adsorbents In General (AREA)
Abstract
The present invention 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,Diode array detector,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,No. 5 mouths of solid-phase extraction column and external six-way valve and No. 7 mouths are connect,No. 14 mouths of six-way valve are connect in No. 9 mouths of One Dimension Analysis column and 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,Two-dimentional trapping column and No. 16 mouths of six-way valve in case,No. 19 mouth connections,No. 18 mouths of two-dimension analysis column and six-way valve in case and diode array detector are connect；This invention simplifies sample pre-treatments operating procedures, improve the analysis efficiency of sample.
Description
[technical field]
The present invention relates to high-efficient liquid phase chromatogram technology field, specifically a kind of bivalve three pumps high-efficient liquid phase color pedigree
System.
[background technology]
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 materia medica, Food Science, environmental monitoring etc..Since the 21th century, chromatography skill
The development of art is gradually ripe, and basic innovation achievement is extremely limited, but technical progress is carrying out always, especially
It is still very active with the relevant action oriented research of industry.
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 pumps and the flow path switching setting between solid-phase extraction column and analytical column realizes 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 and two analytical columns it
Between flow path switching setting realize vitamin A, D, E single injected samplings while, is detected.But since method pre-treatment still needs to saponification
Extraction concentration and etc., pretreatment process very complicated takes consumption manpower, largely effects on the analysis efficiency of sample.
[invention content]
A kind of pump of bivalve three highly effective liquid phase chromatographic system is provided present invention aim to solve above-mentioned deficiency, energy
Enough it is applied to vitamin A in milk powder, the content measuring of D, E, and greatly simplifies sample pre-treatments operating procedure, saves people
Power and reagent cost significantly improve the analysis efficiency of sample.
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 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 the first valve port 14 in case,
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,
In, the Solid Phase Extraction sampling pump 1 is connect with autosampler 2, the absorption for realizing sample analysis solution and sample introduction；It is described
2 other end of autosampler is connect with external first valve port 4 of external six-way valve 3；11 both ends of the solid-phase extraction column respectively with
External second valve port 5 of external six-way valve 3 and the connection of external 4th valve port 7, positive flow path is for realizing sample analysis solution
Primary purification, reversed flow path for realizing enrichment of analyte elution sample introduction；The waste collecting device 10 is logical with external six
The external third valve port 6 of valve 3 connects, for collecting eluent；The One Dimension Analysis pump 12 and the external 5th of external six-way valve 3
Valve port 8 connects, and balancing each other for transport flowing One Dimension Analysis column 13 and reversely elutes and be enriched in the object of solid-phase extraction column 11；
Described 13 one end of One Dimension Analysis column is connect with external 6th valve port 9 of external six-way valve 3, in 13 other end of One Dimension Analysis column and case
First valve port 14 connects in the case of six-way valve 25, is used for analysis part object；The variable-wavelenght detector 20 and in case six
Second valve port 15 connects in the case of port valve 25, for detecting object；22 both ends of the two dimension trapping column are logical in case six respectively
6th valve port 19 connection in third valve port 16 and case in the case of valve 25, positive flow path for realizing enrichment of analyte elution into
Sample, reversed flow path for realizing sample analysis solution double purification；The case of the two-dimension analysis pump 21 and six-way valve 25 in case
The connection of interior 4th valve port 17, for transport, flowing balances each other two-dimension analysis column 23 and positive elute is enriched in two-dimentional trapping column 22
Object；Described 23 one end of two-dimension analysis column is connect with the 5th valve port 18 in the case of six-way valve in case 25, the two-dimension analysis column
23 other ends are connect with diode array detector 24, for detecting object.
Further, further include control system, the control system is 2.2 chromatography data systems of OPENLAB CDS.
Further, when solid-phase extraction column 11 is in loading state, One Dimension Analysis column 13, two-dimentional trapping column 22 and two dimension
Analytical column 23 is in equilibrium state, and 3 flow path of external six-way valve is set as：2→4→5→7→6→10；12→8→9→13；Case
25 flow path of interior six-way valve is set as：13→14→15→20；21→17→16→19→18→23.
Further, when solid-phase extraction column 11 is in elution state, object is transferred to one-dimensional chromatographic column, two dimension capture
Column 22 and two-dimension analysis column 23 are in equilibrium state, and 3 flow path of external six-way valve is set as：12→8→7→5→9→13；2→4
→6→10；25 flow path of six-way valve is set as in case：13→14→15→20；21→17→16→19→18→23.
Further, when solid-phase extraction column 11, which is in, washes down state, object is eluted from one-dimensional chromatographic column, two dimension capture
Column 22 and two-dimension analysis column 23 are in equilibrium state, and 3 flow path of external six-way valve is set as：2→4→5→7→6→10；12→8
→9→13；25 flow path of six-way valve is set as in case：13→14→15→20；21→17→16→19→18→23.
Further, when solid-phase extraction column 11, which is in, washes down state, partial target object is transferred to two from one-dimensional chromatographic column
Trapping column 22 is tieed up, two-dimension analysis column 23 is in equilibrium state, and 3 flow path of external six-way valve is set as：2→4→5→7→6→10；
12→8→9→13；25 flow path of six-way valve is set as in case：21→17→18→23；13→14→19→16→15→20.
Further, when solid-phase extraction column 11 is in equilibrium state, partial target object is transferred to from two-dimentional trapping column 22
Two-dimension analysis column 23, One Dimension Analysis column 13 are in equilibrium state, and 3 flow path of external six-way valve is set as：2→4→5→7→6→10；
12→8→9→13；25 flow path of six-way valve is set as in case：13→14→15→20；21→17→16→19→18→23.
The present invention also provides a kind of highly effective liquid phase chromatographic systems pumped equipped with bivalve three to measure vitamin A in milk powder, D, E
Method, include the following steps：
1) sample treatment：By powdered milk sample mixing, appropriate, addition water, absolute ethyl alcohol, ascorbic acid, BHT and KOH are weighed
Aqueous solution, heats saponification, and postcooling constant volume is completed in saponification；
2) using equipped with bivalve three pump system high performance liquid chromatograph determination step 1) obtained by solution in whether contain
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 present invention compared with the existing technology, has the following advantages that：
(1) present invention establishes a kind of being pumped, it can be achieved that on-line solid phase extraction equipped with bivalve three for a variety of separating mechanisms of combination
The highly effective liquid phase chromatographic system of purification and analysis, and it is applied to vitamin A in milk powder, the content measuring of D, E, single injected sampling
It detects simultaneously, simplifies operating procedure, greatly shorten the time of pre-treatment, save manpower and reagent cost, realize that automatic on-line is net
Change detection, improve sensitivity, ensure the accuracy and reproducibility of test result, from source prevent vitamin enrichment dosage be not allowed to
The adverse effect that consumer health brings.
(2) present invention passes through Solid Phase Extraction to pump the highly effective liquid phase chromatographic system of four root chromatogram columns of connection equipped with bivalve three
With highly effective liquid phase chromatographic system on-line joining process purification and the Two way chromatograms of sample solution are realized in combination with column switching technique
The automatic connection of analysis；Solid-phase extraction column in-line purification analytical solution, one-dimensional chromatography partial target object, Two way chromatograms analysis
Partial target object；Meanwhile trapping column has been used in Two way chromatograms for the first time, it efficiently solves and is distributed in Two way chromatograms due to object
In action process caused by diffusion phenomena the problem of chromatographic peak wide sensitivity decrease.
(3) it after object is enriched in decontaminating column and trapping column in the present invention, is all made of and purification process flow path opposite direction
The mode of elution, object is transferred in analytical column, and the chromatographic peak of acquisition, peak width is moderate, and symmetry is good.
(4) chromatographic column filler used in the present invention is the substance of resistance to highly basic.
(5) present invention is successfully applied in vitamin A in milk powder, during D, E while measures, after the direct constant volume of saponification liquor
Upper machine analysis greatly simplifies sample pre-treatments operation step the step of cleverly avoiding organic solvent phase inversion, concentration, redissolve
Suddenly, the analysis efficiency of sample is significantly improved.Simultaneously as pretreatment process simplifies, vitamin A is reduced, D, E is in analytic process
The risk of middle oxidative degradation, it is ensured that the accuracy and reproducibility of test result.
[description of the drawings]
Analytical solution flow path schematic diagram when Fig. 1 is SPE loadings of the present invention；
Fig. 2 is SPE elutions of the present invention, analytical solution flow path schematic diagram when object is transferred to one-dimensional chromatographic column；
Fig. 3 is SPE cleanings of the present invention, analytical solution flow path schematic diagram when partial target object is eluted from one-dimensional chromatographic column；
Fig. 4 is SPE cleanings of the present invention, and analytical solution flow path shows when partial target object is transferred to trapping column from one-dimensional chromatographic column
It is intended to；
Fig. 5 is SPE of the present invention balance, partial target object from trapping column transfer be two-dimension analysis column when analytical solution flow path show
It is intended to；
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 implementation mode]
The present invention provides a kind of combination a variety of separating mechanisms equipped with the pump of bivalve three four root chromatogram columns of connection, it can be achieved that
Line Solid phase extraction and the bivalve of analysis three pump highly effective liquid phase chromatographic system, including Solid Phase Extraction sampling pump 1, autosampler
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 wavelength
Detector 20, two-dimension analysis pump 21, two-dimentional trapping column 22, two-dimension analysis column 23, diode array detector 24, six-way valve in case
25 and control system, external six-way valve 3 is equipped with external first valve port 4, external second valve port 5, external third valve port 6, external
4th valve port 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 in case in case
Third valve port 16 in two valve ports 15, 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 is connect with autosampler 2, the absorption for realizing sample analysis solution and sample introduction；2 other end of autosampler with
External first valve port 4 of external six-way valve 3 connects；11 both ends of solid-phase extraction column respectively with external second valve of external six-way valve 3
Mouthfuls 5 and the connection of external 4th valve port 7, for realizing the primary purification of sample analysis solution, reversed flow path is used for positive flow path
Realize the elution sample introduction of enrichment of analyte；Waste collecting device 10 is connect with the external third valve port 6 of external six-way valve 3, is used for
Collect eluent；One Dimension Analysis pump 12 and external 5th valve port 8 of external six-way valve 3 connect, and balance each other for transport flowing one-dimensional
Analytical column 13 and reversed elution are enriched in the object of solid-phase extraction column 11；13 one end of One Dimension Analysis column and external six-way valve 3
External 6th valve port 9 connection, 13 other end of One Dimension Analysis column is connect with the first valve port 14 in the case of six-way valve in case 25, for dividing
Analyse partial target object；Variable-wavelenght detector 20 is connect with the second valve port 15 in the case of six-way valve in case 25, for detecting target
Object；22 both ends of two-dimentional trapping column 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,
Positive flow path for realizing enrichment of analyte elution sample introduction, reversed flow path for realizing sample analysis solution double purification；
Two-dimension analysis pump 21 is connect with the 4th valve port 17 in the case of six-way valve in case 25, flows the two-dimension analysis column 23 that balances each other for transporting
The object of two-dimentional trapping column 22 is enriched in positive elution；23 one end of two-dimension analysis column and the in the case of six-way valve 25 in case the 5th
Valve port 18 connects, and 23 other end of two-dimension analysis column is connect with diode array detector 24, for detecting object；Control system
For OPENLAB CDS2.2 chromatography data systems.
Wherein, control system is OPENLAB CDS 2.2, is established using between control platform and power supply system and each device
Connection and communication, test method, test logic, criterion are compiled into testing process software, by control test system come
Replacement personnel operate, and are tested using the automatic testing process.
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, 3 flow path of external six-way valve are set as：2→4→5→7→6→10；12→8→9→13；25 flow path of six-way valve is set in case
It is set to：13→14→15→20；21→17→16→19→18→23.
When solid-phase extraction column elution is in state, object is transferred to one-dimensional chromatographic column, two-dimentional trapping column and two dimension point
Analysis column is in equilibrium state, and 3 flow path of external six-way valve is set as：12→8→7→5→9→13；2→4→6→10；Six in case
25 flow path of port valve is set as：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, and 3 flow path of external six-way valve is set as：2→4→5→7→6→10；12→8→9→13；Six in case
25 flow path of port valve is set as：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, and 3 flow path of external six-way valve is set as：2→4→5→7→6→10；12→8→9→13；Case
25 flow path of interior six-way valve is set as：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, and 3 flow path of external six-way valve is set as：2→4→5→7→6→10；12→8→9→13；Case
25 flow path of interior six-way valve is set as：13→14→15→20；21→17→16→19→18→23.
The present invention is successfully applied to vitamin A in milk powder, and the test of D, E pass through Solid Phase Extraction and high-efficient liquid phase color pedigree
System on-line joining process realizes the automatic connection of the purification and Two way chromatograms analysis of sample solution.One-dimensional chromatography partial target
Object, Two way chromatograms analysis part object.Trapping column has been used for the first time in Two way chromatograms simultaneously, has been efficiently solved due to object
The wide sensitivity decrease of chromatographic peak caused by diffusion phenomena during chromatography distribution behavior the problem of.
The highly effective liquid phase chromatographic system of the present invention pumped equipped with bivalve three measures vitamin A in milk powder, the side of D, E
Method includes the following steps：
1) sample treatment：By powdered milk sample mixing, appropriate, addition water, absolute ethyl alcohol, ascorbic acid, BHT and KOH are weighed
Aqueous solution, heats saponification, and postcooling constant volume is completed in saponification.
2) using equipped with bivalve three pump system high performance liquid chromatograph determination step 1) obtained by solution in whether contain
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 present invention is simultaneously not limited to the embodiments described above, other any Spirit Essences and principle without departing from the present invention
Changes, modifications, substitutions, combinations, simplifications made by lower, should be equivalent substitute mode, be included in the protection model of the present invention
Within enclosing.
Claims (8)
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 row 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) in case, wherein
The Solid Phase Extraction sampling pump (1) connect with autosampler (2), for realizing sample analysis solution absorption and into
Sample；
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, forward stream
Road for realizing sample analysis solution primary purification, reversed flow path for realizing enrichment of analyte elution sample introduction；
The waste collecting device (10) connect with the external third valve port (6) of external six-way valve (3), for collecting eluent；
The One Dimension Analysis pump (12) connect with external 5th valve port (8) of external six-way valve (3), balances each other for transporting flowing
One Dimension Analysis column (13) and reversed elution are enriched in the object of solid-phase extraction column (11)；
Described One Dimension Analysis column (13) one end is connect with external 6th valve port (9) of external six-way valve (3), One Dimension Analysis column (13)
The other end is connect with the first valve port (14) in the case of six-way valve in case (25), is used for analysis part object；
The variable-wavelenght detector (20) connect with the second valve port (15) in the case of six-way valve in case (25), for detecting target
Object；
It is described two dimension trapping column (22) both ends respectively with the 6th valve in third valve port (16) in the case of six-way valve in case (25) and case
Mouthful (19) connection, for positive flow path for realizing the elution sample introduction of enrichment of analyte, reversed flow path is molten for realizing sample analysis
The double purification of liquid；
The two-dimension analysis pump (21) connect with the 4th valve port (17) in the case of six-way valve in case (25), equal for transporting flowing
Weighing apparatus two-dimension analysis column (23) and positive elution are enriched in the object of two-dimentional trapping column (22)；
Described two-dimension analysis column (23) one end is connect with the 5th valve port (18) in the case of six-way valve in case (25), the two-dimension analysis
Column (23) other end is connect with diode array detector (24), for detecting object.
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 systems of CDS.
3. the system as claimed in claim 1, it is characterised in that：When solid-phase extraction column (11) is in loading state, one-dimensional point
Analysis column (13), two-dimentional trapping column (22) and two-dimension analysis column (23) are in equilibrium state, and external six-way valve (3) flow path is set as：2
→4→5→7→6→10；12→8→9→13；Six-way valve (25) flow path is set as in case：13→14→15→20；21→17
→16→19→18→23。
4. the system as claimed in claim 1, it is characterised in that：When solid-phase extraction column (11) is in elution state, object
It is transferred to one-dimensional chromatographic column, two-dimentional trapping column (22) and two-dimension analysis column (23) are in equilibrium state, external six-way valve (3) flow path
It is set as：12→8→7→5→9→13；2→4→6→10；Six-way valve (25) flow path is set as in case：13→14→15→
20；21→17→16→19→18→23.
5. the system as claimed in claim 1, it is characterised in that：When solid-phase extraction column (11), which is in, washes down state, object
It is eluted from one-dimensional chromatographic column, two-dimentional trapping column (22) and two-dimension analysis column (23) are in equilibrium state, external six-way valve (3) flow path
It is set as：2→4→5→7→6→10；12→8→9→13；Six-way valve (25) flow path is set as in case：13→14→15→
20；21→17→16→19→18→23.
6. the system as claimed in claim 1, it is characterised in that：When solid-phase extraction column (11), which is in, washes down state, part mesh
Mark object is transferred to two-dimentional trapping column (22) from one-dimensional chromatographic column, and two-dimension analysis column (23) is in equilibrium state, external six-way valve (3)
Flow path is set as：2→4→5→7→6→10；12→8→9→13；Six-way valve (25) flow path is set as in case：21→17→18
→23；13→14→19→16→15→20.
7. the system as claimed in claim 1, it is characterised in that：When solid-phase extraction column (11) is in equilibrium state, part mesh
Mark object is transferred to two-dimension analysis column (23) from two-dimentional trapping column (22), and One Dimension Analysis column (13) is in equilibrium state, and external six is logical
Valve (3) flow path is set as：2→4→5→7→6→10；12→8→9→13；Six-way valve (25) flow path is set as in case：13→14
→15→20；21→17→16→19→18→23.
8. a kind of bivalve three as described in any one of claim 1 to 7 pumps highly effective liquid phase chromatographic system and measures dimension life in milk powder
Plain A, D, the method for E, which is characterized in that include the following steps：
1) sample treatment：By powdered milk sample mixing, weighs in right amount, it is water-soluble that water, absolute ethyl alcohol, ascorbic acid, BHT and KOH is added
Liquid, heats saponification, and postcooling constant volume is completed in saponification；
2) using equipped with bivalve three pump system high performance liquid chromatograph determination step 1) obtained by solution in whether containing dimension life
Plain A, D, E：If one-dimensional liquid chromatography results show that sample is doubtful containing vitamin A, when E, then comparative sample and vitamin A, E marks
The retention time of quasi- substance, whether to contain vitamin in confirmatory sample
A,E；If two-dimensional liquid chromatography show sample it is doubtful containing vitamin D when, comparative sample and vitamin D standard substance
Retention time, whether to contain vitamin D in confirmatory sample；
If 3) contain vitamin A in confirmatory sample, D, E then calculate vitamin A in sample, the content of D, E by formula.
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| CN110031573A (en) * | 2019-05-31 | 2019-07-19 | 福建省食品药品质量检验研究院 | The method of two-dimensional columns switching high effective liquid chromatography for measuring vitamin D content |
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| CN116618106A (en) * | 2023-07-21 | 2023-08-22 | 深圳赛陆医疗科技有限公司 | Fluid transportation system with variable flow direction, detection system and fluid transportation method thereof |
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