CN102445503A - Combined analytic device for subcritical fluid extraction-liquid chromatography (LC) - Google Patents
Combined analytic device for subcritical fluid extraction-liquid chromatography (LC) Download PDFInfo
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- CN102445503A CN102445503A CN201110282685XA CN201110282685A CN102445503A CN 102445503 A CN102445503 A CN 102445503A CN 201110282685X A CN201110282685X A CN 201110282685XA CN 201110282685 A CN201110282685 A CN 201110282685A CN 102445503 A CN102445503 A CN 102445503A
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Abstract
The invention discloses a combined analytic device for subcritical fluid extraction-liquid phase chromatography (SPE-LC). The combined analytic device comprises an R134a storage tank, two purifiers, a condenser, a high-pressure pump, a heat exchanger, three preheaters, an extraction kettle, a separation kettle, a throttling device, a six-way valve, a cleaning pump, a solid phase catcher, an LC pump, an LC column, a UV (Ultraviolet) detector, a data acquisition unit, a flow meter, a coarse filter, two purifiers, a compressor, six pressure meters, two pressure control displays, seven temperature control displays, a conveying pump, a solvent buffering tank, a two-way valve, a four-way valve, two one-way valves, a current limiting valve, fifteen adjusting valves, an exhaust valve and two waste liquor bottles, wherein the extraction kettle is sealed with a sealing ring; the separation kettle is sealed with a sealing ring; and the outlet of the extraction kettle is connected with the inlet of the separation kettle and an SFE-LC interface through the four-way valve. The device is suitable for analyzing hormone residues of animals, feeds, chemical products, cosmetics and the like, and has the advantages of short analytic time, small using amount of chemical reagents, convenience for operating, recycling of subcritical fluids, low energy consumption and capability of fulfilling the aim of detecting quickly and efficiently.
Description
Technical field
The present invention relates to a kind of subcritical fluid extraction-liquid chromatography combined analysis device, exactly is exactly to adopt R134a fluid under the subcritical state as extractant, from sample, extracts residual sex hormone, carries out the device of online or offline inspection then.
Background technology
Because the long-term usability hormone of people, cause the medicament residue phenomenon that exceeds standard commonplace, the quality problems of food, cosmetics etc. become increasingly conspicuous.Medicament residue directly has influence on the quality of product and consumers in general's health, so forbid in animal feed, foods and cosmetics etc., to add sex hormone in the world wide at present, its detection method is also corresponding grows up.
Continuing to optimize and being gradually improved along with modern chromatographic technique and application of gas chromatorgraphy/mass technology; The work of the test section of sex hormone residual quantity is more and more simplified; Usually analyzing a sample only needs a few minutes to dozens of minutes, and the sample preparation before analyzing needs several hrs.Therefore, the sample pre-treatments technology more and more becomes key and the development priority in the sex hormone retention analysis process, also is the main contents that this problem is intended research.Method about the sex hormone retention analysis also is in the traditional extraction method stage both at home and abroad, comprises liquid-liquid extraction method (LLE), accelerated solvent extraction (ASE), SPE (SPE) and supercritical CO at present
2Extraction etc.But these methods waste time and energy, conventional organic solvents extraction especially, and consumption of organic solvent is big, and is seriously polluted, is unfavorable for operating personnel's health.Supercritical CO
2A series of significant advantages such as efficient height, selectivity are good though extraction has, environmental protection, also exist simultaneously on-stream pressure height, equipment manufacturing cost big, shortcoming such as be difficult for applying.
Because 1,1,1,2-HFC-134a (R134a) has critical condition (Tc=101.1 ℃ Pc=4.06MPa) is easy to reach, low toxicity, inertia, nonflammable and characteristics such as do not damage the ozone layer, so become the first-selection of subcritical fluids.According to literature search, up to the present still do not have and adopt the report of subcritical R134a extraction as the pretreatment technology of sex hormone retention analysis sample, there is not the document of online detection yet, more there is not corresponding device thereof.
Summary of the invention
The invention discloses a kind of subcritical fluid extraction-liquid chromatography combined analysis device; It has low temperature, nontoxic, flow process is simple, easy to operate; In extraction process, realize simultaneously separating; Producers and environment are had no adverse effects, solved prior art length analysis time, contaminated environment, problem such as operator ' s health is unfavorable.
The technical solution adopted for the present invention to solve the technical problems is:
A kind of subcritical fluid extraction-liquid chromatography combined analysis device, it comprises: R134a storage tank (1), clarifier (2), condenser (3), high-pressure pump (4), heat interchanger (5), primary heater (6), extraction kettle (7), separating still (8), flow controller (9), six-way valve (10), scavenging pump (11), solid phase drip catcher (12), LC pump (13), LC chromatographic column (14), UV detecting device (15), data acquisition unit (16), flowmeter (17), coarse filter (18), clarifier (19), compressor (20) is characterized in that: said R134a storage tank (1) is furnished with tensimeter; Variable valve (22) and variable valve (24) are arranged between said R134a storage tank (1) and the filtrator, temperature regulator (26) and variable valve (27) are arranged between said condenser (3) and the high-pressure pump (4), an end of said heat interchanger (5) links to each other with solvent surge tank (28); Said primary heater (6) has temperature control display (35), retaining valve (26) and variable valve (37) to the path of extraction kettle, said extraction kettle (7) is furnished with temperature control display (39), pressure control display (40), tensimeter (41) and variable valve (38), and said separating still is furnished with tensimeter (46), pressure control display (47), temperature control display (48) and variable valve (53); Said extraction kettle (7) is to having variable valve (43), four-way valve (44), tensimeter (49) and variable valve (45) between the said separating still (8), said flow controller (9) one ends are connected to two-port valve, an end is connected to six-way valve (10), and an end is connected to solid phase drip catcher (12); Said six-way valve (10) links to each other with flow controller (9), scavenging pump (11), LC pump (13), LC chromatographic column (14), solid phase drip catcher (12) and waste liquid bottle (55); Between said six-way valve (10) and the waste liquid bottle (55) variable valve (56) is arranged, said scavenging pump (11) links to each other with six-way valve (10), and said solid phase drip catcher (12) one ends are connected to throttling valve; One end is connected to six-way valve (10); Said LC pump links to each other with six-way valve (10), and said LC chromatographic column (14) one ends are connected to six-way valve (10), and an end is connected to UV detecting device (15); Said UV detecting device (15) one ends are connected to data acquisition unit (16); One end is connected to waste liquid bottle (54), and said data acquisition unit (16) links to each other with UV detecting device (15), and tensimeter (60) and variable valve (59) are arranged between said flowmeter (17) and the six-way valve (10); Between said flowmeter (17) and the separating still (8) tensimeter (60) is arranged; Between said coarse filter (18) and the compressor (20) clarifier (19) is arranged, said compressor (20) is connected with tensimeter (61), variable valve (62), vent valve (63), retaining valve (25) and variable valve (27) to the path of high-pressure pump (4), and said compressor (20) is connected with tensimeter (61), variable valve (62), vent valve (63) to the path of R134a storage tank (1); Variable valve (23) and variable valve (22); Said extraction kettle (7) has chuck, and pump (29), primary heater (32), temperature control display (33) and variable valve (34) are arranged between chuck one end and the solvent surge tank (28), and the other end links to each other with separating still (8); Said separating still (8) has chuck; The chuck of separating still (8) has primary heater (50), temperature control display (52) and variable valve (51) to the path of the chuck of extraction kettle (7), said compressor (20) has chuck, and the chuck two ends are connected with solvent conduit; Flow controller (31) and temperature controller (30) are arranged between one end of chuck and the heat interchanger (5); Said extraction kettle (7) seals with O-ring seal, and separating still (8) seals with O-ring seal, and the exit seal place of extraction kettle (7) is connected with (8) of separating still inlet.Both can on-line monitoring with this device, also can offline inspection, when carrying out online detection, close variable valve (45), when carrying out offline inspection, close variable valve (42).
The invention has the beneficial effects as follows:
Through a kind of subcritical fluid extraction disclosed by the invention-liquid chromatography combined analysis device, but robotization control is short to the sex hormone retention analysis time, extracts to detect once and accomplishes.For some special sex hormone, can carry out offline inspection.Whole process operation is convenient, the R134a reusable edible, and less energy consumption, the heat that compressor produces not only can be given the preheating of R134a fluid, and unnecessary heat can also be given extraction kettle and separating still heating.
Description of drawings
Accompanying drawing 1 is the system flowchart of a kind of subcritical fluid extraction of the present invention-liquid chromatography combined analysis device;
Accompanying drawing 2 is schematic diagrams of a kind of subcritical fluid extraction of the present invention-liquid chromatography combined analysis device.
In accompanying drawing 1:
The 1st, R134a storage tank, the 2nd, clarifier, the 3rd, condenser, the 4th, high-pressure column pump, the 5th, heat interchanger, the 6th, primary heater, the 7th, extraction kettle; The 8th, separating still, the 9th, flow controller, the 10th, six-way valve, the 11st, scavenging pump, the 12nd, solid phase drip catcher, the 13rd, LC pump, the 14th, LC chromatographic column; The 15th, UV detecting device, the 16th, data acquisition unit, the 17th, flowmeter, the 18th, coarse filter, the 19th, clarifier, the 20th, compressor, the 21st, tensimeter; The 22nd, variable valve, the 23rd, variable valve, the 24th, variable valve, the 25th, retaining valve, the 26th, temperature control display, the 27th, variable valve, the 28th, surge tank; The 29th, pump, the 30th, temperature control display, the 31st, flow controller, the 32nd, primary heater, the 33rd, temperature control display, the 34th, variable valve, the 35th, temperature control display; The 36th, retaining valve, the 37th, variable valve, the 38th, variable valve, the 39th, temperature control display, the 40th, pressure control display, the 41st, tensimeter, the 42nd, variable valve; The 43rd, variable valve, the 44th, four-way valve, the 45th, variable valve, the 46th, tensimeter, the 47th, pressure control display, the 48th, temperature control display, the 49th, tensimeter; The 50th, primary heater, the 51st, be variable valve, the 52nd, temperature control display, the 53rd, variable valve, the 54th, waste liquid bottle, the 55th, waste liquid bottle, the 56th, variable valve; The 57th, variable valve, the 58th, two-port valve, the 59th, variable valve, the 60th, tensimeter, the 61st, tensimeter, the 62nd, variable valve, the 63rd, vent valve.
Embodiment:
In order to simplify the technological process that the sample hormone residues is analyzed; Cut down the consumption of energy; Shorten the time of whole workflow; Thereby alleviate analyst's labour intensity, and can pollution-free high-efficient carry out the residual analytical work of sample sex hormone, the invention provides a kind of subcritical fluid extraction-liquid chromatography combined analysis device.When subcritical fluids contacts with analytic sample; Optionally dissolve residual hormone wherein; Mode through decompression and intensification makes subcritical fluids reply normality and volatilization rapidly then; Dissolved sex hormone is just separated out with solid-state form, can carry out online or offline inspection then, thereby reaches the residual purpose of analytic sample sex hormone.
In accompanying drawing 1; A kind of subcritical fluid extraction-liquid chromatography combined analysis device; It comprises: R134a storage tank (1), clarifier (2), condenser (3), high-pressure pump (4), heat interchanger (5), primary heater (6), extraction kettle (7), separating still (8), flow controller (9), six-way valve (10), scavenging pump (11), solid phase drip catcher (12), LC pump (13), LC chromatographic column (14), UV detecting device (15), data acquisition unit (16), flowmeter (17), coarse filter (18), clarifier (19), compressor (20); It is characterized in that: said R134a storage tank (1) is furnished with tensimeter (21); Variable valve (22) and variable valve (24) are arranged between said R134a storage tank (1) and the filtrator; Temperature regulator (26) and variable valve (27) are arranged between said condenser (3) and the high-pressure pump (4); One end of said heat interchanger (5) links to each other with solvent surge tank (28); Said primary heater (6) has temperature control display (35), retaining valve (26) and variable valve (37) to the path of extraction kettle (7); Said extraction kettle (7) is furnished with temperature control display (39), pressure control display (40), tensimeter (41) and variable valve (38); Said separating still is furnished with tensimeter (46), pressure control display (47), temperature control display (48) and variable valve (53), and said extraction kettle (7) is to having variable valve (43), four-way valve (44), tensimeter (49) and variable valve (45) between the said separating still (8), and said flow controller (9) one ends are connected to two-port valve, an end is connected to six-way valve (10); One end is connected to solid phase drip catcher (12); Said six-way valve (10) links to each other with flow controller (9), scavenging pump (11), LC pump (13), LC chromatographic column (14), solid phase drip catcher (12), flowmeter (17) and waste liquid bottle (55), between said six-way valve (10) and the waste liquid bottle (55) variable valve (56) is arranged, and said scavenging pump (11) links to each other with six-way valve (10); Said solid phase drip catcher (12) one ends are connected to throttling valve; One end is connected to six-way valve (10), said LC pump and six-way valve (10) and links to each other, and said LC chromatographic column (14) one ends are connected to six-way valve (10), and an end is connected to UV detecting device (15); Said UV detecting device (15) one ends are connected to data acquisition unit (16); One end is connected to waste liquid bottle (54), and said data acquisition unit (16) links to each other with UV detecting device (15), between said flowmeter (17) and the separating still (8) tensimeter (63) is arranged; Tensimeter (60) and variable valve (59) are arranged between said flowmeter (17) and the six-way valve (10); Between said coarse filter (18) and the compressor (20) clarifier (19) is arranged, said compressor (20) is connected with tensimeter (61), variable valve (62), vent valve (63), retaining valve (25) and regulator (27) to the path of high-pressure pump (4), and said compressor (20) is connected with tensimeter (61), variable valve (62), vent valve (63), variable valve (23) and variable valve (22) to the path of R134a storage tank (1).
Said extraction kettle (7) has chuck, and pump (29), primary heater (32), temperature control display (33) and variable valve (34) are arranged between chuck one end and the solvent surge tank (28), and the other end links to each other with separating still (8).Said separating still (8) has chuck, and the chuck of separating still (8) has primary heater (50), temperature control display (52) and variable valve (51) to the path of extraction kettle chuck.Said compressor (20) has chuck, and the chuck two ends are connected with solvent conduit, and flow controller (31) and temperature controller (30) are arranged between an end of chuck and the heat interchanger (5).Said extraction kettle (7) seals with O-ring seal, and separating still (8) seals with O-ring seal, and the exit seal place of extraction kettle (7) is connected with (8) of separating still inlet.Both can on-line monitoring with this device, also can offline inspection, when carrying out online detection, close variable valve (45), when carrying out offline inspection, close variable valve (42).
Concrete principle of work is following:
R134a in the R134a storage tank 1 is sent in the condenser 3 after purifying through clarifier 2; Condenser 3 is frozen into liquid with R134a again, is transported to by high-pressure pump 4 and carries out preliminary preheating in the heat interchanger 5, is transported to then in the primary heater 6; Be heated to form subcritical fluids with uniform temperature; Entering is heated in the extraction kettle 7 of uniform temperature, contacts with wherein sample, optionally the residual hormone in the sample dissolution.If carry out online detection, then close variable valve 45, open variable valve 42 and two-port valve 58; The R134a fluid that is dissolved with hormone enters into the lower solid phase drip catcher 12 of pressure through flow controller 9, because pressure reduces, solubleness descends; Solute among the R134a is separated out, and by 12 absorption of solid phase drip catcher, R134a gets into coarse filter 18 through variable valve 59 and flowmeter 17 and purifies with clarifier 19; Be sent to compression in the compressor 20 then, be sent in the high-pressure pump 4 recycle then through variable valve 62, retaining valve 25 and variable valve 27; After extraction is accomplished, start LC chromatogram pump 13, elute the hormone of solid phase drip catcher 12 absorption; Be sent in the LC chromatographic column 14 and separate, be sent at last in the UV detecting device 15 and detect, data are by data acquisition unit 16 collection analysises; If carry out offline inspection, then close variable valve 42, open variable valve 45; Be dissolved with the lower separating still 8 of R134a fluid input pressure of hormone, because pressure reduces, solubleness descends; Solute among the R134a is separated out, and stays in the separating still 8, and R134a gets into successively in coarse filter 18 and the clarifier 19 through variable valve 57 and flowmeter 17 and purifies; Be sent to compression in the compressor 20 then, the R134a fluid after the compression is sent in the high-pressure pump 4 through variable valve 62, retaining valve 25 and variable valve 27, recycle; After extraction is accomplished, can carry out offline inspection to the hormone in the separating still 8.In order to reduce energy consumption, in whole extraction process, the heat that compressor produces is taken to by water carries out preliminary preheating in the heat interchanger 5 the R134a fluid; Hot water after the heat exchange is sent in the solvent surge tank 28; Pump 29 is sent in the primary heater 32 then, and the hot water that is heated to uniform temperature is sent in the chuck of extraction kettle 7 through variable valve 34, gives the insulation of R134a fluid; When carrying out offline inspection; The hot water that in the chuck of extraction kettle 7, flows out is sent to the primary heater 50, and the hot water that is heated to uniform temperature is sent in the chuck of separating still 8 through variable valve 51, gives separating still 8 insulations.
Claims (11)
1. subcritical fluid extraction-liquid chromatography combined analysis device; It comprises: R134a storage tank (1), clarifier (2), condenser (3), high-pressure column pump (4), be heat interchanger (5), primary heater (6), extraction kettle (7), separating still (8), flow controller (9), six-way valve (10), scavenging pump (11), solid phase drip catcher (12), LC pump (13), LC chromatographic column (14), UV detecting device (15), data acquisition unit (16), flowmeter (17), coarse filter (18), clarifier (19), compressor (20); It is characterized in that: said R134a storage tank (1) is furnished with tensimeter (21); Variable valve (22) and variable valve (24) are arranged between said R134a storage tank (1) and the filtrator; Temperature regulator (26) and variable valve (27) are arranged between said condenser (3) and the high-pressure pump (4); One end solvent surge tank (28) of said heat interchanger (5); Said primary heater (6) has temperature control display (35), retaining valve (26) and variable valve (37) to the path of extraction kettle; Said extraction kettle (7) is furnished with temperature control display (39), pressure control display (40), tensimeter (41) and variable valve (38); Said separating still is furnished with tensimeter (46), pressure control display (47), temperature control display (48) and variable valve (53); Said extraction kettle (7) is to variable valve (43), four-way valve (44), tensimeter (49) and variable valve (45) are arranged between the said separating still (8); Said flow controller (9) one ends are connected to two-port valve, an end is connected to six-way valve (10), and an end is connected to solid phase drip catcher (12), and said six-way valve (10) links to each other with flow controller (9), scavenging pump (11), LC pump (13), LC chromatographic column (14), solid phase drip catcher (12), flowmeter (17) and waste liquid bottle (55); Between said six-way valve (10) and the waste liquid bottle (55) variable valve (56) is arranged; Said scavenging pump (11) links to each other with six-way valve (10), and said solid phase drip catcher (12) one ends are connected to throttling valve, and an end is connected to six-way valve (10), said LC pump and six-way valve (10) and links to each other; Said LC chromatographic column (14) one ends are connected to six-way valve (10); One end is connected to UV detecting device (15), and said UV detecting device (15) one ends are connected to data acquisition unit (16), and an end is connected to waste liquid bottle (54); Said data acquisition unit (16) links to each other with UV detecting device (15); Between said flowmeter (17) and the separating still (8) tensimeter (63) is arranged, tensimeter (60) and variable valve (59) are arranged between said flowmeter (17) and the six-way valve (10), between said coarse filter (18) and the compressor (20) clarifier is arranged; Said compressor (20) is connected with tensimeter (61), variable valve (62), vent valve (63), retaining valve (25) and regulator (27) to the path of high-pressure pump (4), said compressor (20) is connected with tensimeter (61), variable valve (62), vent valve (63), variable valve (23) and variable valve (24) to the path of clarifier (2).
2. a kind of subcritical fluid extraction according to claim 1-liquid chromatography combined analysis device, it is characterized in that: used subcritical fluids is R134a.
3. a kind of subcritical fluid extraction according to claim 1-liquid chromatography combined analysis device; It is characterized in that: said extraction kettle (7) has chuck; Pump (29), primary heater (32), temperature control display (33) and variable valve (34) are arranged between chuck one end and the solvent surge tank (28), and the other end links to each other with separating still (8).
4. a kind of subcritical fluid extraction according to claim 1-liquid chromatography combined analysis device is characterized in that: said separating still (8) has chuck.
5. according to claim 3 and 4 described a kind of subcritical fluid extraction-liquid chromatography combined analysis devices, it is characterized in that: the chuck of separating still has primary heater (50), temperature control display (52) and variable valve (51) on the set pattern of the chuck of extraction kettle.
6. a kind of subcritical fluid extraction according to claim 1-liquid chromatography combined analysis device; It is characterized in that: said compressor (20) has chuck; The chuck two ends are connected with solvent conduit, and flow controller (31) and temperature controller (30) are arranged between an end of chuck and the heat interchanger (5).
7. a kind of subcritical fluid extraction according to claim 6-liquid chromatography combined analysis device is characterized in that: used fluid is a water in the solvent conduit at compressor chuck two ends.
8. a kind of subcritical fluid extraction according to claim 1-liquid chromatography combined analysis device is characterized in that: both can on-line monitoring with this device, and also can offline inspection.
9. a kind of subcritical fluid extraction according to claim 1-liquid chromatography combined analysis device; It is characterized in that: extraction kettle (7) seals with O-ring seal; Separating still (8) seals with O-ring seal, and the exit seal place of extraction kettle (7) is connected with (8) of separating still inlet.
10. a kind of subcritical fluid extraction according to claim 1-liquid chromatography combined analysis device is characterized in that: when carrying out online detection, close variable valve (45).
11. a kind of subcritical fluid extraction according to claim 1-liquid chromatography combined analysis device is characterized in that: when carrying out offline inspection, close variable valve (42).
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| CN102757861A (en) * | 2012-07-31 | 2012-10-31 | 青岛海康水产发展有限公司 | Method for extracting sea cucumber lipids |
| CN102879257A (en) * | 2012-10-12 | 2013-01-16 | 上海爱吉伦光谱仪器有限公司 | Full-automatic fast solvent extraction-solid phase extraction spectrometer and extraction method thereof |
| CN107121504A (en) * | 2017-04-12 | 2017-09-01 | 岛津企业管理（中国）有限公司 | Multi-functional temperature-pressure extraction trapping chromatographic isolation on-line coupling equipment |
| CN108532187A (en) * | 2018-06-22 | 2018-09-14 | 中原工学院 | A kind of subcritical fluids non-aqueous dyeing method and apparatus |
| CN108614055A (en) * | 2017-12-30 | 2018-10-02 | 青岛袁策生物科技有限公司 | A kind of high performance liquid chromatography pretreating device |
| CN110291392A (en) * | 2017-02-13 | 2019-09-27 | 株式会社岛津制作所 | Super critical fluid apparatus |
| CN110393945A (en) * | 2019-09-04 | 2019-11-01 | 睿科集团(厦门)股份有限公司 | A kind of multichannel pressure extraction flow path and its extracting process |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102757861A (en) * | 2012-07-31 | 2012-10-31 | 青岛海康水产发展有限公司 | Method for extracting sea cucumber lipids |
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| CN102879257B (en) * | 2012-10-12 | 2015-11-04 | 上海爱吉伦光谱仪器有限公司 | A kind of full-automatic Accelerate solvent extraction-Solid-Phase Extraction combined instrument and extracting process thereof |
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| CN108614055A (en) * | 2017-12-30 | 2018-10-02 | 青岛袁策生物科技有限公司 | A kind of high performance liquid chromatography pretreating device |
| CN108532187A (en) * | 2018-06-22 | 2018-09-14 | 中原工学院 | A kind of subcritical fluids non-aqueous dyeing method and apparatus |
| CN108532187B (en) * | 2018-06-22 | 2024-01-26 | 亚临界(上海)技术有限公司 | Subcritical fluid anhydrous dyeing method and subcritical fluid anhydrous dyeing equipment |
| CN110393945A (en) * | 2019-09-04 | 2019-11-01 | 睿科集团(厦门)股份有限公司 | A kind of multichannel pressure extraction flow path and its extracting process |
| CN110393945B (en) * | 2019-09-04 | 2024-03-08 | 睿科集团(厦门)股份有限公司 | Multichannel pressurized extraction flow path and extraction method thereof |
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