CN107884506A - A kind of liquid chromatography system - Google Patents
A kind of liquid chromatography system Download PDFInfo
- Publication number
- CN107884506A CN107884506A CN201710978229.6A CN201710978229A CN107884506A CN 107884506 A CN107884506 A CN 107884506A CN 201710978229 A CN201710978229 A CN 201710978229A CN 107884506 A CN107884506 A CN 107884506A
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- regulating valve
- valve
- separating still
- pressure gauge
- control display
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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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
-
- 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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N2030/8804—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 automated systems
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- 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
A kind of liquid chromatography system, by a kind of subcritical fluid extraction liquid chromatogram combined analysis device disclosed by the invention, can Automated condtrol, short to the sex hormone retention analysis time, extraction detection is once completed.For some special sex hormone, offline inspection can be carried out.Whole process is easy to operate, R134a reusable edibles, less energy consumption, and heat caused by compressor can not only give R134a fluids to preheat, and unnecessary heat can also give extraction kettle and separating still to heat.
Description
Technical field
The present invention relates to a kind of subcritical fluid extraction-liquid chromatogram combined analysis device, is exactly exactly using sub-
R134a fluids under critical condition extract the sex hormone of residual from sample, then carry out online or offline inspection as extractant
The device of survey.
Background technology
Due to people's long-term use sex hormone, cause the exceeded phenomenon of medicament residue commonplace, the matter of food, cosmetics etc.
Amount problem becomes increasingly conspicuous.Medicament residue has directly influenced the quality of product and the health of consumers in general, so the current world
In the range of forbid to add sex hormone in animal feed, foods and cosmetics etc., its detection method is also accordingly grown up.
Continuing to optimize and being gradually improved with modern chromatographic techniques and application of gas chromatorgraphy/mass technology, the inspection of sex hormone residual quantity
The work for surveying part increasingly simplifies, and generally analyzing a sample only needs a few minutes to dozens of minutes, and at the sample before analyzing
Reason but needs several hours.Therefore, Sample Pretreatment Technique increasingly becomes the key and hair during sex hormone retention analysis
Emphasis is opened up, and this problem intends the main contents of research.The method on sex hormone retention analysis extracts also in tradition both at home and abroad
The method stage is taken, at present including liquid-liquid extraction method (LLE), accelerated solvent extraction (ASE), SPE (SPE) and overcritical
CO2 extractions etc..But these methods waste time and energy, especially conventional organic solvents extraction, consumption of organic solvent is big, and pollution is tight
Weight, it is unfavorable for the health of operating personnel.Although SCF-CO 2 has efficiency high, selectivity good, green etc. a series of
The advantages of notable.
The content of the invention
The invention discloses a kind of subcritical fluid extraction-liquid chromatogram combined analysis device, its have low temperature, it is nontoxic,
Flow is simple and convenient to operate, and realizes separation simultaneously in extraction process, producers and environment are had no adverse effects, solved
Prior art analysis time is long, pollution environment, it is unfavorable to operator's health the problems such as.
A kind of subcritical fluids R134a extractions-liquid chromatogram combined analysis device, it includes：R134a storage tanks (1), first
Clarifier (2), condenser (3), high-pressure pump (4), heat exchanger (5), preheater (6), extraction kettle (7), separating still (8), flow controller
(9), six-way valve (10), cleaning pump (11), solid phase trap (12), LC pumps (13), LC chromatographic columns (14), UV detectors (15),
Data acquisition unit (16), flowmeter (17), coarse filter (18), the second clarifier (19), compressor (20), it is characterised in that：
The R134a storage tanks (1) are furnished with pressure gauge, have the first regulating valve between the R134a storage tanks (1) and the first clarifier (2)
(22) and the 3rd regulating valve (24), there are thermoregulator (26) and the 4th regulating valve between the condenser (3) and high-pressure pump (4)
(27), one end of the heat exchanger (5) is connected with solvent surge tank (28), has on the preheater (6) to the path of extraction kettle
Temperature control display (35), check valve (36) and the 6th regulating valve (37), the extraction kettle (7) are furnished with temperature control display
(39), Stress control display (40), pressure gauge (41) and the 7th regulating valve (38), the separating still equipped with pressure gauge (46),
Stress control display (47), temperature control display (48) and the 12nd regulating valve (53), the extraction kettle (7) is to described point
From having the 9th regulating valve (43), four-way valve (44), pressure gauge (49) and the tenth regulating valve (45), the flow controller between kettle (8)
(9) one end is connected to two-port valve, one end is connected to six-way valve (10), and one end is connected to solid phase trap (12), with flow controller (9)
The other end of the connected two-port valve in one end is connected with the 8th regulating valve (42), the six-way valve (10) and flow controller (9), cleaning pump
(11), LC pumps (13), LC chromatographic columns (14), solid phase trap (12) are connected with waste liquid bottle (55), the six-way valve (10) and useless
There is the 13rd regulating valve (56) between liquid bottle (55), the cleaning pump (11) is connected with six-way valve (10), the solid phase trap
(12) one end is connected to flow controller (9), and one end is connected to six-way valve (10), the LC pumps are connected with six-way valve (10), the LC
Chromatographic column (14) one end is connected to six-way valve (10), and one end is connected to UV detectors (15), and described UV detectors (15) one end connects
Data acquisition unit (16) is connected to, one end is connected to waste liquid bottle (54), and one end is connected to LC chromatographic columns (14), the data acquisition unit
(16) it is connected with UV detectors (15), there is pressure gauge (60) and the 15th regulation between the flowmeter (17) and six-way valve (10)
Valve (59), there are pressure gauge (60) and the 14th regulating valve (57), the coarse filtration between the flowmeter (17) and separating still (8)
There is the second clarifier (19) between device (18) and compressor (20), be connected with the compressor (20) to the path of high-pressure pump (4)
Pressure gauge (61), the 16th regulating valve (62), air bleeding valve (63), check valve (25) and the 4th regulating valve (27), the compressor
(20) to being connected with pressure gauge (61), the 16th regulating valve (62), air bleeding valve (63), the second regulating valve on the path of R134a (1)
And the first regulating valve (22) (23).The extraction kettle (7) carries chuck, has pump between chuck one end and solvent surge tank (28)
(29), preheater (32), temperature control display (33) and the 5th regulating valve (34), the other end are connected with separating still (8).It is described
Separating still (8) carries chuck, has preheater (50), temperature control on the chuck of separating still (8) to the path of the chuck of extraction kettle
Display (52) processed and the 11st regulating valve (51).The compressor (20) carries chuck, and chuck both ends are connected with solvent conduit, folder
There are flow controller (31) and temperature controller (30) between one end of set and heat exchanger (5).Extraction kettle (7) is carried out close with sealing ring
Envelope, separating still (8) are sealed with sealing ring, are connected at the exit seal of extraction kettle (7) with (8) entrance of separating still.With
This device can both be monitored on-line, can also offline inspection, when conducting on-line testing, the tenth regulating valve (45) is closed, when entering
During row offline inspection, the 8th regulating valve (42) is closed.
The beneficial effects of the invention are as follows：
By a kind of subcritical fluid extraction-liquid chromatogram combined analysis device disclosed by the invention, can Automated condtrol, to property
Hormone residues analysis time is short, and extraction detection is once completed.For some special sex hormone, offline inspection can be carried out.Entirely
Process operation is convenient, R134a reusable edibles, less energy consumption, and heat caused by compressor can not only give R134a fluids to preheat,
And unnecessary heat can also give extraction kettle and separating still to heat.
Brief description of the drawings
Accompanying drawing 1 is a kind of system flow chart of subcritical fluid extraction-liquid chromatogram combined analysis device of the present invention；
Accompanying drawing 2 is a kind of schematic diagram of subcritical fluid extraction-liquid chromatogram combined analysis device of the present invention.
In fig. 1：
1 is R134a storage tanks, and 2 be the first clarifier, and 3 be condenser, and 4 be high-pressure column pump, and 5 be heat exchanger, and 6 be preheater, and 7 are
Extraction kettle, 8 be separating still, and 9 be flow controller, and 10 be six-way valve, and 11 be cleaning pump, and 12 be solid phase trap, and 13 be LC pumps, and 14 are
LC chromatographic columns, 15 be UV detectors, and 16 be data acquisition unit, and 17 be flowmeter, and 18 be coarse filter, and 19 be the second clarifier,
20 be compressor, and 21 be pressure gauge, and 22 be the first regulating valve, and 23 be the second regulating valve, and 24 be the 3rd regulating valve, and 25 be unidirectional
Valve, 26 be temperature control display, and 27 be the 4th regulating valve, and 28 be surge tank, and 29 be pump, and 30 be temperature control display, 31
It is flow controller, 32 be preheater, and 33 be temperature control display, and 34 be the 5th regulating valve, and 35 be temperature control display, and 36 are
Check valve, 37 be the 6th regulating valve, and 38 be the 7th regulating valve, and 39 be temperature control display, and 40 be Stress control display, 41
It is pressure gauge, 42 be the 8th regulating valve, and 43 be the 9th regulating valve, and 44 be four-way valve, and 45 be the tenth regulating valve, and 46 be pressure gauge,
47 be Stress control display, and 48 be temperature control display, and 49 be pressure gauge, and 50 be preheater, and 51 be the 11st regulating valve,
52 be temperature control display, and 53 be the 12nd regulating valve, and 54 be waste liquid bottle, and 55 be waste liquid bottle, and 56 be the 13rd regulating valve, 57
It is the 14th regulating valve, 58 be two-port valve, and 59 be the 15th regulating valve, and 60 be pressure gauge, and 61 be pressure gauge, and 62 be the 16th tune
Valve is saved, 63 be air bleeding valve.
Embodiment：
In order to simplify the technological process of sample hormone residues analysis, energy consumption is reduced, shortens the time of whole workflow, from
And mitigate the labor intensity of analysis personnel, and can be with the analysis work of the progress sample sex hormone residual of pollution-free high-efficient, this
Invention provides a kind of subcritical fluid extraction-liquid chromatogram combined analysis device.When subcritical fluids and analysis sample contact
When, residual sex hormone therein is optionally dissolved, subcritical fluids is replied normality by way of depressurizing and heating up
And volatilize rapidly, dissolved sex hormone just separates out in solid form, online or offline inspection then can be carried out, so as to reach
Analyze the purpose of sample sex hormone residual.
In fig. 1, a kind of subcritical fluids R134a extractions-liquid chromatogram combined analysis device, it includes：R134a is stored up
Tank (1), the first clarifier (2), condenser (3), high-pressure pump (4), heat exchanger (5), preheater (6), extraction kettle (7), separating still
(8), flow controller (9), six-way valve (10), cleaning pump (11), solid phase trap (12), LC pumps (13), LC chromatographic columns (14), UV inspections
Device (15), data acquisition unit (16), flowmeter (17), coarse filter (18), the second clarifier (19), compressor (20) are surveyed, its
It is characterised by：The R134a storage tanks (1) are furnished with pressure gauge (21), between the R134a storage tanks (1) and the first clarifier (2)
First has regulating valve (22) and the 3rd regulating valve (24), has thermoregulator (26) between the condenser (3) and high-pressure pump (4)
With the 4th regulating valve (27), one end of the heat exchanger (5) is connected with solvent surge tank (28), the preheater (6) to extraction
There are temperature control display (35), check valve (36) and the 6th regulating valve (37) on the path of kettle (7), the extraction kettle (7) is matched somebody with somebody
There are temperature control display (39), Stress control display (40), pressure gauge (41) and the 7th regulating valve (38), the separating still
Equipped with pressure gauge (46), Stress control display (47), temperature control display (48) and the 12nd regulating valve (53), the extraction
Kettle (7) is taken to having the 9th regulating valve (43), four-way valve (44), pressure gauge (49) and the tenth regulating valve between the separating still (8)
(45), described flow controller (9) one end is connected to two-port valve, one end is connected to six-way valve (10), and one end is connected to solid phase trap
(12) other end for the two-port valve, being connected with flow controller (9) one end is connected with the 8th regulating valve (42), the six-way valve (10) and
Flow controller (9), cleaning pump (11), LC pumps (13), LC chromatographic columns (14), solid phase trap (12) are connected with waste liquid bottle (55), institute
Stating has the 13rd regulating valve (56) between six-way valve (10) and waste liquid bottle (55), the cleaning pump (11) and six-way valve (10) phase
Even, described solid phase trap (12) one end is connected to flow controller (9), and it is logical that one end is connected to six-way valve (10), the LC pumps and six
Valve (10) is connected, and described LC chromatographic columns (14) one end is connected to six-way valve (10), and one end is connected to UV detectors (15), the UV
Detector (15) one end is connected to data acquisition unit (16), and one end is connected to LC chromatographic columns (14), and one end is connected to waste liquid bottle
(54), one end is connected to LC chromatographic columns (14), and the data acquisition unit (16) is connected with UV detectors (15), the flowmeter
(17) have pressure gauge (60) between separating still (8), have between the flowmeter (17) and six-way valve (10) pressure gauge (60) and
15th regulating valve (59), there are the second clarifier (19), the compressor between the coarse filter (18) and compressor (20)
(20) to being connected with pressure gauge (61), the 16th regulating valve (62), air bleeding valve (63), check valve (25) on the path of high-pressure pump (4)
With the 4th regulating valve (27), pressure gauge (61) is connected with the compressor (20) to the path of R134a storage tanks (1), the 16th is adjusted
Save valve (62), air bleeding valve (63), the second regulating valve (23) and the first regulating valve (22).
The extraction kettle (7) carries chuck, there is pump (29), preheater between chuck one end and solvent surge tank (28)
(32), temperature control display (33) and the 5th regulating valve (34), the other end are connected with separating still (8).Separating still (8) band
There is a chuck, have preheater (50), temperature control display (52) and the tenth on the chuck of separating still to the path of extraction kettle chuck
One regulating valve (51).The compressor (20) carries chuck, and chuck both ends are connected with solvent conduit, one end of chuck and heat exchanger
(5) there are flow controller (31) and temperature controller (30) between.The extraction kettle (7) is sealed with sealing ring, and separating still (8) is used
Sealing ring is sealed, and is connected at the exit seal of extraction kettle (7) with (8) entrance of separating still.Both can be with this device
Line monitor, can also offline inspection, when conducting on-line testing, close the tenth regulating valve (45), when carrying out offline inspection,
Close the 8th regulating valve (42).
Claims (6)
1. a kind of liquid chromatography system, it is characterised in that it includes：R134a storage tanks (1), the first clarifier (2), condensation
Device (3), high-pressure pump (4), heat exchanger (5), preheater (6), extraction kettle (7), separating still (8), flow controller (9), six-way valve (10),
Cleaning pump (11), solid phase trap (12), LC pumps (13), LC chromatographic columns (14), UV detectors (15), data acquisition unit (16),
Flowmeter (17), coarse filter (18), the second clarifier (19), compressor (20), it is characterised in that：The R134a storage tanks (1)
Equipped with pressure gauge, there are the first regulating valve (22) and the 3rd regulating valve between the R134a storage tanks (1) and the first clarifier (2)
(24), there are thermoregulator (26) and the 4th regulating valve (27), the heat exchanger between the condenser (3) and high-pressure pump (4)
(5) one end is connected with solvent surge tank (28), has temperature control display on the preheater (6) to the path of extraction kettle
(35), check valve (36) and the 6th regulating valve (37), the extraction kettle (7) is equipped with temperature control display (39), Stress control
Display (40), pressure gauge (41) and the 7th regulating valve (38), the separating still is equipped with pressure gauge (46), Stress control display
(47), temperature control display (48) and the 12nd regulating valve (53), the extraction kettle (7) have between the separating still (8)
9th regulating valve (43), four-way valve (44), pressure gauge (49) and the tenth regulating valve (45), described flow controller (9) one end are connected to
Two-port valve, one end are connected to six-way valve (10), and one end is connected to solid phase trap (12), two to be connected with flow controller (9) one end
The other end of port valve is connected with the 8th regulating valve (42), the six-way valve (10) and flow controller (9), cleaning pump (11), LC pumps
(13), LC chromatographic columns (14), solid phase trap (12) are connected with waste liquid bottle (55), the six-way valve (10) and waste liquid bottle (55) it
Between have the 13rd regulating valve (56), the cleaning pump (11) is connected with six-way valve (10), and described solid phase trap (12) one end connects
Flow controller (9) is connected to, one end is connected to six-way valve (10), the LC pumps are connected with six-way valve (10), the LC chromatographic columns (14)
One end is connected to six-way valve (10), and one end is connected to UV detectors (15), and described UV detectors (15) one end is connected to data and adopted
Storage (16), one end are connected to waste liquid bottle (54), and one end is connected to LC chromatographic columns (14), the data acquisition unit (16) and UV inspections
Survey device (15) to be connected, have pressure gauge (60) and the 15th regulating valve (59), institute between the flowmeter (17) and six-way valve (10)
Stating has pressure gauge (60) and the 14th regulating valve (57) between flowmeter (17) and separating still (8), the coarse filter (18) and
There is the second clarifier (19) between compressor (20), pressure gauge is connected with the compressor (20) to the path of high-pressure pump (4)
(61), the 16th regulating valve (62), air bleeding valve (63), check valve (25) and the 4th regulating valve (27), the compressor (20) are arrived
Be connected with pressure gauge (61), the 16th regulating valve (62), air bleeding valve (63) on R134a (1) path, the second regulating valve (23) and
First regulating valve (22).
2. a kind of liquid chromatography system according to claim 1, it is characterised in that the extraction kettle (7) is with folder
Set, there are pump (29), preheater (32), temperature control display (33) and the 5th to adjust between chuck one end and solvent surge tank (28)
Valve (34) is saved, the other end is connected with separating still (8).
3. a kind of liquid chromatography system according to claim 1, it is characterised in that the separating still (8) is with folder
Set, there are preheater (50), temperature control display (52) and the on the chuck of separating still (8) to the path of the chuck of extraction kettle
11 regulating valves (51).
4. a kind of liquid chromatography system according to claim 1, it is characterised in that the compressor (20) is with folder
Set, chuck both ends are connected with solvent conduit, there is flow controller (31) and temperature controller between one end of chuck and heat exchanger (5)
(30)。
5. a kind of liquid chromatography system according to claim 1, it is characterised in that extraction kettle (7) is entered with sealing ring
Row sealing, separating still (8) are sealed with sealing ring, are connected at the exit seal of extraction kettle (7) with (8) entrance of separating still
Connect.
6. a kind of liquid chromatography system according to claim 1, it is characterised in that can both have been supervised online with this device
Survey, can also offline inspection, when conducting on-line testing, close the tenth regulating valve (45), when carrying out offline inspection, closing the
Eight regulating valves (42).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710978229.6A CN107884506A (en) | 2017-10-19 | 2017-10-19 | A kind of liquid chromatography system |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710978229.6A CN107884506A (en) | 2017-10-19 | 2017-10-19 | A kind of liquid chromatography system |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107884506A true CN107884506A (en) | 2018-04-06 |
Family
ID=61781931
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710978229.6A Pending CN107884506A (en) | 2017-10-19 | 2017-10-19 | A kind of liquid chromatography system |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107884506A (en) |
-
2017
- 2017-10-19 CN CN201710978229.6A patent/CN107884506A/en active Pending
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| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20180406 |
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| WD01 | Invention patent application deemed withdrawn after publication |