CN102445503B - 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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- CN102445503B CN102445503B CN201110282685.XA CN201110282685A CN102445503B CN 102445503 B CN102445503 B CN 102445503B CN 201110282685 A CN201110282685 A CN 201110282685A CN 102445503 B CN102445503 B CN 102445503B
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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, is exactly exactly to adopt R134a fluid under subcritical state as extractant, extracts residual sex hormone from sample, then carries out the device of online or offline inspection.
Background technology
Due to 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 to add sex hormone in world wide in animal feed, foods and cosmetics etc. at present, its detection method is corresponding growing up also.
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, conventionally analyzing a sample only needs a few minutes to dozens of minutes, and sample preparation before analyzing needs several hours.Therefore, Sample Pretreatment Technique more and more becomes key and the development priority in sex hormone retention analysis process, is also the main contents that this problem is intended research.The domestic and international method about sex hormone retention analysis, also in the traditional extraction method stage, comprises liquid-liquid extraction method (LLE), accelerated solvent extraction (ASE), Solid-Phase Extraction (SPE) and supercritical CO at present
2extraction etc.But these methods waste time and energy, especially conventional organic solvents extraction, consumption of organic solvent is large, seriously polluted, is unfavorable for operating personnel's health.Supercritical CO
2although extraction has a series of significant advantages such as efficiency is high, selectivity good, environmental protection, also exist the shortcomings such as on-stream pressure is high, equipment manufacturing cost large, be difficult for applying simultaneously.
Because HFA 134a (R134a) has that critical condition (Tc=101.1 DEG C, Pc=4.06MPa) is easy to reach, low toxicity, inertia, the nonflammable and feature such as do not damage the ozone layer, so become the first-selection of subcritical fluids.According to literature search, up to the present there is no and adopt the report of subcritical R134a extraction as the pretreatment technology of sex hormone retention analysis sample, there is no the online document detecting, more without corresponding device yet.
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 and separating simultaneously, producers and environment are had no adverse effects, solved prior art length analysis time, contaminated environment, to the 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 fluids R134a extraction-liquid chromatography combined analysis device, it comprises: R134a storage tank (1), the first 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), the second clarifier (19), compressor (20), it is characterized in that: described R134a storage tank (1) is furnished with tensimeter, between described R134a storage tank (1) and the first clarifier (2), there are the first variable valve (22) and the 3rd variable valve (24), between described condenser (3) and high-pressure pump (4), there are temperature regulator (26) and the 4th variable valve (27), one end of described heat interchanger (5) is connected with solvent surge tank (28), described primary heater (6) has temperature control display (35) to the path of extraction kettle, retaining valve (36) and the 6th variable valve (37), described extraction kettle (7) is furnished with temperature control display (39), pressure control display (40), tensimeter (41) and the 7th variable valve (38), described separating still is furnished with tensimeter (46), pressure control display (47), temperature control display (48) and the 12 variable valve (53), described extraction kettle (7) is to there being the 9th variable valve (43) between described separating still (8), four-way valve (44), tensimeter (49) and the tenth variable valve (45), described flow controller (9) one end is connected to two-port valve, one end is connected to six-way valve (10), one end is connected to solid phase drip catcher (12), the other end of the two-port valve being connected with flow controller (9) one end is connected with the 8th variable valve (42), described six-way valve (10) and flow controller (9), scavenging pump (11), LC pump (13), LC chromatographic column (14), solid phase drip catcher (12) is connected with waste liquid bottle (55), between described six-way valve (10) and waste liquid bottle (55), there is the 13 variable valve (56), described scavenging pump (11) is connected with six-way valve (10), described solid phase drip catcher (12) one end is connected to flow controller (9), one end is connected to six-way valve (10), described LC pump is connected with six-way valve (10), described LC chromatographic column (14) one end is connected to six-way valve (10), one end is connected to UV detecting device (15), described UV detecting device (15) one end is connected to data acquisition unit (16), one end is connected to waste liquid bottle (54), one end is connected to LC chromatographic column (14), described data acquisition unit (16) is connected with UV detecting device (15), between described flowmeter (17) and six-way valve (10), there are tensimeter (60) and the 15 variable valve (59), between described flowmeter (17) and separating still (8), there are tensimeter (60) and the 14 variable valve (57), between described coarse filter (18) and compressor (20), there is the second clarifier (19), described compressor (20) is connected with tensimeter (61) to the path of high-pressure pump (4), the 16 variable valve (62), vent valve (63), retaining valve (25) and the 4th variable valve (27), described compressor (20) is connected with tensimeter (61) to the path of R134a (1), the 16 variable valve (62), vent valve (63), the second variable valve (23) and the first variable valve (22).Described extraction kettle (7) is with chuck, between chuck one end and solvent surge tank (28), have pump (29), primary heater (32), temperature control display (33) and the 5th variable valve (34), the other end is connected with separating still (8).Described separating still (8) is with chuck, and the chuck of separating still (8) has primary heater (50), temperature control display (52) and the 11 variable valve (51) to the path of the chuck of extraction kettle.Described compressor (20) is with chuck, and chuck two ends are connected with solvent conduit, has flow controller (31) and temperature controller (30) between one end of chuck and heat interchanger (5).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) entrance of separating still.With this device both can on-line monitoring, also can offline inspection, in the time detecting online, close the tenth variable valve (45), in the time carrying out offline inspection, close the 8th variable valve (42).
The invention has the beneficial effects as follows:
By a kind of subcritical fluid extraction-liquid chromatography combined analysis device disclosed by the invention, can robotization control, short to the sex hormone retention analysis time, extract to detect and once complete.For some special sex hormone, can carry out offline inspection.Whole process operation is convenient, 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.
Brief description of the drawings
Accompanying drawing 1 is the system flowchart of a kind of subcritical fluid extraction-liquid chromatography of the present invention combined analysis device;
Accompanying drawing 2 is schematic diagrams of a kind of subcritical fluid extraction-liquid chromatography of the present invention combined analysis device.
In accompanying drawing 1:
The 1st, R134a storage tank, 2 is first clarifiers, 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, 19 is second clarifiers, the 20th, compressor, the 21st, tensimeter, 22 is first variable valve, 23 is second variable valve, 24 is the 3rd variable valve, the 25th, retaining valve, the 26th, temperature control display, 27 is the 4th 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, 34 is the 5th variable valve, the 35th, temperature control display, the 36th, retaining valve, 37 is the 6th variable valve, 38 is the 7th variable valve, the 39th, temperature control display, the 40th, pressure control display, the 41st, tensimeter, 42 is the 8th variable valve, 43 is the 9th variable valve, the 44th, four-way valve, 45 is the tenth variable valve, the 46th, tensimeter, the 47th, pressure control display, the 48th, temperature control display, the 49th, tensimeter, the 50th, primary heater, 51 is the 11 variable valve, the 52nd, temperature control display, 53 is the 12 variable valve, the 54th, waste liquid bottle, the 55th, waste liquid bottle, 56 is the 13 variable valve, 57 is the 14 variable valve, the 58th, two-port valve, 59 is the 15 variable valve, the 60th, tensimeter, the 61st, tensimeter, 62 is the 16 variable valve, the 63rd, vent valve.
embodiment:
The technological process of analyzing in order to simplify sample hormone residues, reduce energy consumption, 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.In the time that subcritical fluids contacts with analytic sample, optionally dissolve residual hormone wherein, then make subcritical fluids reply normality volatilization rapidly by the mode that reduces pressure and heat up, dissolved sex hormone is just separated out with solid-state form, then can carry out online or offline inspection, thereby reach the residual object of analytic sample sex hormone.
In accompanying drawing 1, a kind of subcritical fluids R134a extraction-liquid chromatography combined analysis device, it comprises: R134a storage tank (1), the first 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), the second clarifier (19), compressor (20), it is characterized in that: described R134a storage tank (1) is furnished with tensimeter (21), between described R134a storage tank (1) and the first clarifier (2), first has variable valve (22) and the 3rd variable valve (24), between described condenser (3) and high-pressure pump (4), there are temperature regulator (26) and the 4th variable valve (27), one end of described heat interchanger (5) is connected with solvent surge tank (28), and described primary heater (6) has temperature control display (35) to the path of extraction kettle (7), retaining valve (36) and the 6th variable valve (37), described extraction kettle (7) is furnished with temperature control display (39), pressure control display (40), tensimeter (41) and the 7th variable valve (38), described separating still is furnished with tensimeter (46), pressure control display (47), temperature control display (48) and the 12 variable valve (53), described extraction kettle (7) is to there being the 9th variable valve (43) between described separating still (8), four-way valve (44), tensimeter (49) and the tenth variable valve (45), described flow controller (9) one end is connected to two-port valve, one end is connected to six-way valve (10), one end is connected to solid phase drip catcher (12), the other end of the two-port valve being connected with flow controller (9) one end is connected with the 8th variable valve (42), described six-way valve (10) and flow controller (9), scavenging pump (11), LC pump (13), LC chromatographic column (14), solid phase drip catcher (12) is connected with waste liquid bottle (55), between described six-way valve (10) and waste liquid bottle (55), there is the 13 variable valve (56), described scavenging pump (11) is connected with six-way valve (10), described solid phase drip catcher (12) one end is connected to flow controller (9), and one end is connected to six-way valve (10), described LC pump is connected with six-way valve (10), described LC chromatographic column (14) one end is connected to six-way valve (10), one end is connected to UV detecting device (15), described UV detecting device (15) one end is connected to data acquisition unit (16), one end is connected to LC chromatographic column (14), one end is connected to waste liquid bottle (54), one end is connected to LC chromatographic column (14), described data acquisition unit (16) is connected with UV detecting device (15), between described flowmeter (17) and separating still (8), there is tensimeter (60), between described flowmeter (17) and six-way valve (10), there are tensimeter (60) and the 15 variable valve (59), between described coarse filter (18) and compressor (20), there is the second clarifier (19), described compressor (20) is connected with tensimeter (61) to the path of high-pressure pump (4), the 16 variable valve (62), vent valve (63), retaining valve (25) and the 4th variable valve (27), described compressor (20) is connected with tensimeter (61) to the path of R134a storage tank (1), the 16 variable valve (62), vent valve (63), the second variable valve (23) and the first variable valve (22).
Described extraction kettle (7) is with chuck, between chuck one end and solvent surge tank (28), have pump (29), primary heater (32), temperature control display (33) and the 5th variable valve (34), the other end is connected with separating still (8).Described separating still (8) is with chuck, and the chuck of separating still has primary heater (50), temperature control display (52) and the 11 variable valve (51) to the path of extraction kettle chuck.Described compressor (20) is with chuck, and chuck two ends are connected with solvent conduit, has flow controller (31) and temperature controller (30) between one end of chuck and heat interchanger (5).Described 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) entrance of separating still.With this device both can on-line monitoring, also can offline inspection, in the time detecting online, close the tenth variable valve (45), in the time carrying out offline inspection, close the 8th variable valve (42).
Specific works principle is as follows:
R134a in R134a storage tank 1 is sent in condenser 3 after clarifier 2 purifies, condenser 3 is frozen into liquid by R134a again, be transported to and in heat interchanger 5, carry out preliminary preheating by high-pressure pump 4, then be transported in primary heater 6, be heated to form the subcritical fluids with uniform temperature, enter in the extraction kettle 7 that is heated to uniform temperature, contact with sample wherein, optionally the residual hormone in sample dissolution.If detected online, close the tenth variable valve 45, open the 8th variable valve 42 and two-port valve 58, the R134a fluid that is dissolved with sex hormone enters into by flow controller 9 the solid phase drip catcher 12 that pressure is lower, due to pressure decreased, solubleness declines, solute in R134a is separated out, adsorbed by solid phase drip catcher 12, R134a is through the 15 variable valve 59 and flowmeter 17 enters coarse filter 18 and clarifier 19 purifies, then be sent to compression in compressor 20, then by the 16 variable valve 62, retaining valve 25 and the 4th variable valve 27 are sent in high-pressure pump 4, recycle, after extraction completes, start LC chromatogram pump 13, the sex hormone that solid phase drip catcher 12 is adsorbed elutes, in the LC chromatographic column 14 of making a gift to someone, separate, finally be sent in UV detecting device 15 and detect, data are by data acquisition unit 16 collection analysises, if carry out offline inspection, close the 8th variable valve 42, open the tenth variable valve 45, be dissolved with the lower separating still 8 of R134a fluid input pressure of sex hormone, due to pressure decreased, solubleness declines, solute in R134a is separated out, stay in separating still 8, R134a enters purification in coarse filter 18 and clarifier 19 successively through the 14 variable valve 57 and flowmeter 17, then be sent to compression in compressor 20, R134a fluid after compression is by the 16 variable valve 62, retaining valve 25 and the 4th variable valve 27 are sent in high-pressure pump 4, recycle, after extraction completes, can carry out offline inspection to the sex hormone in separating still 8.In order to reduce energy consumption, in whole extraction process, the heat that compressor produces is taken in heat interchanger 5 and is carried out preliminary preheating to R134a fluid by water, hot water after heat exchange is sent in solvent surge tank 28, then pump 29 is sent in primary heater 32, the hot water that is heated to uniform temperature is sent in the chuck of extraction kettle 7 through the 5th variable valve 34, give the insulation of R134a fluid, in the time carrying out offline inspection, the hot water flowing out in the chuck of extraction kettle 7 is sent to primary heater 50, the hot water that is heated to uniform temperature is sent in the chuck of separating still 8 through the 11 variable valve 51, be incubated to separating still 8.
Claims (9)
1. a subcritical fluids R134a extraction-liquid chromatography combined analysis device, it comprises: R134a storage tank (1), the first 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), the second clarifier (19), compressor (20), it is characterized in that: described R134a storage tank (1) is furnished with tensimeter (21), between described R134a storage tank (1) and the first clarifier (2), there are the first variable valve (22) and the 3rd variable valve (24), between described condenser (3) and high-pressure pump (4), there are temperature regulator (26) and the 4th variable valve (27), one end of described heat interchanger (5) is connected with solvent surge tank (28), described primary heater (6) has temperature control display (35) to the path of extraction kettle, retaining valve (36) and the 6th variable valve (37), described extraction kettle (7) is furnished with temperature control display (39), pressure control display (40), tensimeter (41) and the 7th variable valve (38), described separating still is furnished with tensimeter (46), pressure control display (47), temperature control display (48) and the 12 variable valve (53), described extraction kettle (7) is to there being the 9th variable valve (43) between described separating still (8), four-way valve (44), tensimeter (49) and the tenth variable valve (45), described flow controller (9) one end is connected to two-port valve, one end is connected to six-way valve (10), one end is connected to solid phase drip catcher (12), the other end of the two-port valve being connected with flow controller (9) one end is connected with the 8th variable valve (42), described six-way valve (10) and flow controller (9), scavenging pump (11), LC pump (13), LC chromatographic column (14), solid phase drip catcher (12) is connected with waste liquid bottle (55), between described six-way valve (10) and waste liquid bottle (55), there is the 13 variable valve (56), described scavenging pump (11) is connected with six-way valve (10), described solid phase drip catcher (12) one end is connected to flow controller (9), one end is connected to six-way valve (10), described LC pump is connected with six-way valve (10), described LC chromatographic column (14) one end is connected to six-way valve (10), one end is connected to UV detecting device (15), described UV detecting device (15) one end is connected to data acquisition unit (16), one end is connected to waste liquid bottle (54), one end is connected to LC chromatographic column (14), described data acquisition unit (16) is connected with UV detecting device (15), between described flowmeter (17) and separating still (8), there are tensimeter (60) and the 14 variable valve (57), between described flowmeter (17) and six-way valve (10), there are tensimeter (60) and the 15 variable valve (59), between described coarse filter (18) and compressor (20), there is the second clarifier (19), described compressor (20) is connected with tensimeter (61) to the path of high-pressure pump (4), the 16 variable valve (62), vent valve (63), retaining valve (25) and the 4th variable valve (27), described compressor (20) is connected with tensimeter (61) to the path of the first clarifier (2), the 16 variable valve (62), vent valve (63), the second variable valve (23) and the 3rd variable valve (24).
2. a kind of subcritical fluids R134a extraction-liquid chromatography combined analysis device according to claim 1, it is characterized in that: described extraction kettle (7) is with chuck, between chuck one end and solvent surge tank (28), have pump (29), primary heater (32), temperature control display (33) and the 5th variable valve (34), the other end is connected with separating still (8).
3. a kind of subcritical fluids R134a extraction-liquid chromatography combined analysis device according to claim 1, is characterized in that: described separating still (8) is with chuck.
4. a kind of subcritical fluids R134a extraction-liquid chromatography combined analysis device according to claim 3, is characterized in that: the chuck of separating still has primary heater (50), temperature control display (52) and the 11 variable valve (51) on the set pattern of the chuck of extraction kettle.
5. a kind of subcritical fluids R134a extraction-liquid chromatography combined analysis device according to claim 1, it is characterized in that: described compressor (20) is with chuck, chuck two ends are connected with solvent conduit, have flow controller (31) and temperature controller (30) between one end of chuck and heat interchanger (5).
6. a kind of subcritical fluids R134a extraction-liquid chromatography combined analysis device according to claim 5, is characterized in that: in the solvent conduit at compressor chuck two ends, fluid used is water.
7. a kind of subcritical fluids R134a extraction-liquid chromatography combined analysis device according to claim 1, 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) entrance of separating still.
8. a kind of subcritical fluids R134a extraction-liquid chromatography combined analysis device according to claim 1, is characterized in that: in the time detecting online, close the tenth variable valve (45).
9. a kind of subcritical fluids R134a extraction-liquid chromatography combined analysis device according to claim 1, is characterized in that: in the time carrying out offline inspection, close the 8th variable valve (42).
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| CN201110282685.XA CN102445503B (en) | 2011-09-22 | 2011-09-22 | Combined analytic device for subcritical fluid extraction-liquid chromatography (LC) |
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| CN201110282685.XA CN102445503B (en) | 2011-09-22 | 2011-09-22 | Combined analytic device for subcritical fluid extraction-liquid chromatography (LC) |
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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 |
| 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 |
| US11243193B2 (en) * | 2017-02-13 | 2022-02-08 | Shimadzu Corporation | Supercritical fluid device |
| CN107121504B (en) * | 2017-04-12 | 2019-08-20 | 岛津企业管理（中国）有限公司 | Multi-functional temperature-pressure extraction-trapping-chromatographic isolation on-line coupling equipment |
| 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 |
| 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 |
| 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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| US5198115A (en) * | 1991-07-09 | 1993-03-30 | Analytical Bio-Chemistry Laboratories, Inc. | Integrated instrument for supercritical fluid sample extraction, sample separation and concentration |
| JP4508778B2 (en) * | 2004-08-20 | 2010-07-21 | ダイセル化学工業株式会社 | Sample injection method, sample injection apparatus, and supercritical fluid chromatography apparatus having the same |
| CN1276251C (en) * | 2005-03-31 | 2006-09-20 | 卢建刚 | Supercritical fluid analog moving bed chromatograph of ternary area |
| CN100581630C (en) * | 2007-12-18 | 2010-01-20 | 华南理工大学 | Ultrasonic reinforced subcritical water extraction method of natural product effective ingredient and device |
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