CN107870219A - A kind of small chemical derivatization device - Google Patents
A kind of small chemical derivatization device Download PDFInfo
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- CN107870219A CN107870219A CN201610848268.XA CN201610848268A CN107870219A CN 107870219 A CN107870219 A CN 107870219A CN 201610848268 A CN201610848268 A CN 201610848268A CN 107870219 A CN107870219 A CN 107870219A
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- derivatization
- pipe
- lower cover
- samming
- heat
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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
- G01N30/62—Detectors specially adapted therefor
- G01N30/74—Optical detectors
Abstract
The invention discloses a kind of small chemical derivatization device.Derivatization reaction pipe elder generation's pre-wound winds the scheme of derivatization reaction pipe instead of traditional netted derivatization device of establishment and on U-shaped heat conductive rod on more short-range missile hot pins.The mode of heating of reaction tube is heated using heat conductive rod directly-heated and the air bath formed by upper and lower two cover plates, makes derivatization reaction pipe homogeneous heating and cold area free, samming error ± 0.2 DEG C；The short stainless steel tube of termination liner of derivatization reaction pipe, reaction tube external application stainless steel cutting ferrule and the sealing of stubborn cap, pressure-resistant seal is more reliable, pressure-resistant reachable 4MPa.The chemically derived device is applied to the On-chip derivatization of the compounds such as aflatoxin, and aflatoxin B1 and G1 fluorescence intensity can be made to improve 6.5 times；It is low, practical that whole chemically derived device average temperature performance is more preferable, derivative efficiency high and performance repeat reliable, compact, heating power consumption.
Description
Technical field
The present invention relates to high performance liquid chromatography (HPLC) detector technologies field, is used to increase more specifically to one kind
The small chemical derivatization device of hyperfluorescence detection signal.The supporting fluorescence detector of derivatization device disclosed by the invention uses, for detecting
During aflatoxin in food, medicinal material and feed, aflatoxin B1 and G1 fluorescence response signal can be significantly improved.
Background technology
Aflatoxin (AFTS) is a kind of molecule mycotoxin, and it is referred to as most strong natural carcinogen, 1993
Aflatoxin is set to I class carcinogenic substance by the Agency for Research on Cancer of the World Health Organization (WHO).Aflatoxin is widely present in
In the cereal product to go mouldy, the aflatoxin detected in agricultural product and food is international major issue.Separate at present
Aflatoxin have kind more than ten, mainly have B1 (AFTB1), B2 (AFB2), G1 (AFTG1), G2 (AFTG2), M1 (AFTM1).
Wherein, B1 toxicity is most strong, is approximately 10 times of potassium cyanide, is 68 times of arsenic trioxide (arsenic).Aflatoxin detection side
Method mainly has High Performance Liquid Chromatography with Fluorescence Detection, fluorimetry, liquid chromatography-mass spectrometry etc..In numerous AFTS national standards
In detection method, propose that the earliest and current method being most widely used is high performance liquid chromatography-fluorescence (HPLC-
FLD) method, such as GB/T 18979-2003 and GB/T 23212-2008.With the developing of epoch, the progress of science and technology, national standard and Europe
Mark gradually reduces to the limitation of aflatoxin in all kinds of materials.
Aflatoxin B1 and G1 inherently stronger fluorescence, but after it is contacted with water, have fluorescent quenching phenomenon hair
Raw, fluorescence becomes very weak, so typically improving their fluorescence intensity with deriving method.Main flow deriving method is after post at present
Iodine/bromine chemistry derivatization method and photochemical derivatization method.Photochemical derivatization method is although simple to operate, but photochemistry in the market is spread out
The excitation source of raw device is all 254nm low pressure mercury lamps, and only 2000-3000 hours in its life-span, as lighting time lengthens, its is gradual
Aging can be such that light intensity gradually reduces, and cause the long-time stability for deriving result bad；Iodine/bromine chemistry derivatization method, while it is desirable to post
Derive pump afterwards, also to prepare derivative liquid, but its long-term derivative stability and repeatability are preferable, and GB/T 18979-2003 foods
Product examine test with Chinese Pharmacopoeia in 2015 as defined in deriving method.Chemically derived device heats because needing, and need to have the property that：(1)
Post efflux and derivative liquid energy enough sufficiently and uniformly mix；(2) derivatization device should provide stabilization, uniformly derive temperature field, and have
There is good heat insulation effect；(3) derivatization device small volume, simple to operate.
The content of the invention：
Pin on the other hand, we have invented it is a it is small-sized, be exclusively used in aflatoxin detection post after iodine/bromine chemistry derivatization device.
Derivatization device is divided into derivatization device core module and lagging casing module.(1) derivatization reaction pipe is uniform, is compactly wrapped in 4 heat conducting pipes
Above, should around tubular construction and method derivatization device more netted than traditional establishment and U-tube winding arrangement more compact, compact；(2)
Heat conducting pipe is heated by lower cover, and heat conducting pipe reheats derivatization reaction pipe；And closed by upper and lower cover plates, include heating core and
The cavity of samming body provides the air bath uniformly heated for derivatization reaction pipe and heat conducting pipe, makes derivatization reaction pipe cold area free, temperature
Degree is evenly distributed.Experiment measures, when whole 8-10m derivatization reaction pipe is heated to 70 DEG C, only ± 0.2 DEG C of samming unevenness.
(3) material of derivatization reaction pipe is PTFE/FEP flexible pipes, and the long stainless steel tubes of 8-10mm are lining into the termination of pipe, after use stainless steel
Cutting ferrule and the sealing of stubborn cap, make pressure-resistant seal more reliable.Experiment measures pressure-resistant 4MPa.(4) it is chemically derived through experiment, patent of the present invention
Device can make aflatoxin B1 and G1 fluorescence intensity improve 6.5 times.
The technical scheme is that：
A kind of small chemical derivatization device, it is characterised in that：Derivatization device is made up of derivatization device core and lagging casing, derivatization device core
Including：Derivatization reaction pipe, heat conducting pipe, lead screw, mixing tee, samming body, heating core, lower cover, temperature sensor, upper lid
Plate, heat-preservation cotton and lagging casing；The lower cover is made up of a plane bottom plate and two perpendicular risers, two riser phases
It is mutually parallel；Derivatization reaction pipe is uniform, is closely wrapped on 2-6 root heat conducting pipes, and lead screw and spiral shell are used in the both ends of heat conducting pipe respectively
Cap is fixed on two risers of lower cover；The heat conducting pipe is metal straight pipe；Samming body is fixed on lower cover by screw
Bottom plate on, is provided with heating core in samming body；Mixing tee is fixed on samming body by screw, and one of mixing tee connects
Mouth is connected with one end of derivatization reaction pipe, and two other interface connects liquid chromatogram column outlet and derivative liquid entrance respectively；It is derivative
The other end of reaction tube is connected to fluorescence detector；Temperature sensor is fixed on the riser of lower cover；The upper cover plate passes through
Screw is fixed together with samming body, and derivatization reaction pipe, heat conducting pipe, samming body and mixing tee are covered, and forms samming
Inner chamber, as derivatization device core；The outside of derivatization device core is provided with heat-preservation cotton, is placed in lagging casing.
The material of the derivatization reaction pipe is polytetrafluoroethylene (PTFE) (PTFE) or fluorinated ethylene propylene copolymer (FEP), pipe range
7-12m, external diameter 1.0-1.6mm, internal diameter 0.3-0.5mm, the both ends intubating length 8-10mm of pipe stainless steel tube, stainless steel tube
External diameter is adapted to the internal diameter of derivatization reaction pipe (1), internal diameter 0.2-0.3mm.
The heat conducting pipe is long 60-110mm, external diameter 6-11mm, internal diameter 3-5mm metal straight pipe.
The mixing tee is the general standard three-way connector of high performance liquid chromatography.
The heat conducting pipe, samming body, the material of lower cover and upper cover plate are the good metallic aluminium of heat conductivility, copper or stainless
Steel.
The material of the heat-preservation cotton is the melamine foamed plastic with compared with low thermal conductivity, glass fibre cotton or ceramic fibre
Cotton.
It is coated between the samming body and lower cover, between heating core and samming body and between mixing tee and samming body
One layer of uniform heat-conducting silicone grease.
Compared with prior art, chemically derived utensil of the invention has the following advantages：
1st, compared to flexible derivatization reaction pipe is woven into web frame and derivatization reaction pipe is wrapped on U-shaped heat conducting pipe
Structure, short straight tube pre-wound derivatization reaction pipe of the invention, average temperature performance is more preferable, derive efficiency high and performance repeats reliable, body
Product is compact, practical.
2nd, derivatization reaction pipe is heated jointly by heat conductive rod+air bath, makes derivatization reaction pipe cold area free, temperature is uniform, entirely
The temperature error of derivative pipe is within ± 0.2 DEG C, and broadening of the chromatographic peak after derivatization device is relatively small, it is also more preferable to go out peak shape.
3rd, short stainless steel tube is lining into the termination of PTFE/FEP derivatization reactions pipe, then is sealed with stainless steel cutting ferrule and stubborn cap,
Make pressure-resistant seal more reliable, pressure-resistant reachable 4MPa.
4th, whole chemically derived device makes aflatoxin B1 and G1 fluorescence intensity improve 6.5 times.
5th, whole chemically derived device derives efficiency high and performance repeats that reliable, compact, heating power consumption be low, practicality
By force.
Brief description of the drawings
Fig. 1 (a) is the view that chemically derived device is not added with upper cover plate, and Fig. 1 (b) is chemically derived device core regarding plus cover plate
Figure, Fig. 1 (c) are plus the overall isometric view of the chemically derived device after lagging casing.In figure：1- derivatization reaction pipes, 2- are led
Heat pipe, 3- lead screw, 4- mixing tees, 5- samming bodies, 6- heating cores, 7- lower covers, 8- temperature sensors, 9- upper cover plates, 10-
Heat-preservation cotton, 11- lagging casings, 301- nuts and 101- stainless steel tubes.
Fig. 2 is the detection spectrogram of embodiment 1.
Embodiment
A kind of small chemical derivatization device, it is characterised in that：Derivatization device is made up of derivatization device core and lagging casing, derivatization device core
Including：Derivatization reaction pipe 1, heat conducting pipe 2, lead screw 3, mixing tee 4, samming body 5, heating core 6, lower cover 7, temperature sensor
8th, upper cover plate 9, heat-preservation cotton 10 and lagging casing 11；The lower cover 7 has a plane bottom plate and two perpendicular riser groups
Into two risers are parallel to each other；Derivatization reaction pipe 1 is uniform, is closely wrapped on 2-6 roots heat conducting pipe 2, the both ends of heat conducting pipe 2
It is fixed on respectively with lead screw 3 and nut 301 on two risers of lower cover 7；The heat conducting pipe 2 is metal straight pipe；Samming body 5
It is fixed on by screw on the bottom plate of lower cover 7, heating core 6 is provided with samming body 5；Mixing tee 4 is fixed by screw
On samming body 5, an interface of mixing tee 4 is connected with one end of derivatization reaction pipe 1, and two other interface connects liquid respectively
Phase column outlet and derivative liquid entrance；The other end of derivatization reaction pipe 1 is connected to fluorescence detector；Temperature sensor 8 is fixed
On the riser of lower cover 7；The upper cover plate 9 is fixed together by screw and samming body 5, and by derivatization reaction pipe 1, lead
Heat pipe 2, samming body 5 and mixing tee 4 cover, and samming inner chamber are formed, as derivatization device core；The outside of derivatization device core is provided with insulation
Cotton 10, it is placed in lagging casing 11.
The material of derivatization reaction pipe 1 is polytetrafluoroethylene (PTFE) (PTFE) or fluorinated ethylene propylene copolymer (FEP), pipe range 7-
12m, external diameter 1.0-1.6mm, internal diameter 0.3-0.5mm, the both ends intubating length 8-10mm of pipe stainless steel tube 101, stainless steel tube
101 external diameter is adapted to the internal diameter of derivatization reaction pipe 1, internal diameter 0.2-0.3mm.
Heat conducting pipe 2 is long 60-110mm, external diameter 6-11mm, internal diameter 3-5mm metal straight pipe.
Mixing tee 4 is the general standard three-way connector of high performance liquid chromatography.
Heat conducting pipe 2, samming body 5, the material of lower cover 7 and upper cover plate 9 are the good metallic aluminium of heat conductivility, copper or stainless
Steel.
The material of heat-preservation cotton 9 is the melamine foamed plastic with compared with low thermal conductivity, glass fibre cotton or ceramic fiber cotton.
All applied between samming body 5 and lower cover 7, between heating core 6 and samming body 5 and between mixing tee 4 and samming body 5
There is one layer of uniform heat-conducting silicone grease.
Embodiment 1
As shown in figure 1, have developed means of iodine chemical derivatization device after small-sized post, derivatization reaction pipe is internal diameter 0.4mm, long 10m it is poly-
Tetrafluoroethene pipe, external diameter 0.5mm, internal diameter 0.25mm, long 9mm stainless steel tube are inserted with two terminations of pipe；Mixing tee
One interface is connected with one end of polytetrafluoroethylene (PTFE), and two other interface accesses two sections of 1/16 inch of external diameters, internal diameter 0.25mm
Stainless steel tube, liquid chromatogram column outlet and derivative liquid are connected respectively.The other end of polyfluortetraethylene pipe is connected to fluorescence detector.
Derivatization device core is wrapped with heat-preservation cotton, is placed in another housing (11).The means of iodine chemical derivatization device and seminar are developed certainly
FD-1200S types fluorescence detector connection evaluate its performance.Liquid phase chromatogram condition：Chromatographic column：C18 posts, 4.6mm × 150mm ×
5μm；Mobile phase A methanol：Mobile phase B pure water=45:55；Flow rate of mobile phase：0.8mL/min；Sample introduction：20 μ L 1.5ppb are yellow bent
The mixed mark of mould toxin.Post-column derivation condition：Derivative liquid：The aqueous solution (adding 10% methanol) of 0.05% iodine；Derivatization device temperature：70℃；
Derivative flow velocity：0.2mL/min.Hangzhou Pu Hui Science and Technology Ltd.s Sepu3010 chromatographic work stations are used for signal acquisition.
Experimental result：
Fig. 2 is detection spectrogram：(1) FD-1200S is used, is not derived, direct injected, aflatoxin B1 detection is limited to
0.14ppb；(2) means of iodine chemical derivatization device of the present invention is used, 6.5 times are improved to the detection sensitivity of aflatoxin B1, test limit
For 0.02ppb.We are tested at the Pribolab KRC Photochemical derivatization devices (Singapore's production) of also commodity in use,
Pribolab KRC Photochemical derivatization devices make B1 sensitivity improve 6.5 times.
It can be seen that what the small-sized means of iodine chemical derivatization device of the present invention produced to B1 fluorescence sensitivity enhancing effect with Singapore
Pribolab KRC Photochemical derivatization devices are identical.Separately test, Pribolab KRC Photochemical derivatization devices are used continuously three months
Afterwards, because the life-span only 2000-3000h of low pressure mercury lamp, its detection sensitivity have started to decline；And the means of iodine chemical that the present invention develops
After derivatization device is used continuously 1 year, the response of its detection sensitivity is still very stable, has no decay.It can be seen that means of iodine chemical of the present invention is spread out
Pribolab KRC Photochemical derivatization device of the stability of raw device also superior to import.
Design philosophy according to the embodiment of the present invention is modified pair to the embodiment and application of embodiment
It is obvious for those skilled in the art.The present invention is not intended to be limited to embodiment illustrated herein, and
It is to fit to the most wide scope consistent with General Principle disclosed herein and features of novelty.It is all to think according to present invention design
The change for any no creative work for wanting to be made is all within protection scope of the present invention.
Claims (8)
- A kind of 1. small chemical derivatization device, it is characterised in that：Derivatization device is made up of derivatization device core and lagging casing, derivatization device core bag Include：Derivatization reaction pipe (1), heat conducting pipe (2), lead screw (3), mixing tee (4), samming body (5), heating core (6), lower cover (7), temperature sensor (8), upper cover plate (9), heat-preservation cotton (10) and lagging casing (11)；The upper cover plate (9) and lower cover (7) It is made up of a square planar bottom plate and two perpendicular risers, two risers are parallel to each other；Derivatization reaction pipe (1) is equal It is even, be closely wrapped on 2-6 roots heat conducting pipe (2), the both ends of heat conducting pipe (2) are respectively with lead screw (3) and nut (301) fixation On two risers of lower cover (7)；The heat conducting pipe (2) is metal straight pipe；Samming body (5) is fixed on lower cover by screw On the bottom plate of plate (7), heating core (6) is provided with samming body (5)；Mixing tee (4) is fixed on samming body (5) by screw On, an interface of mixing tee (4) is connected with one end of derivatization reaction pipe (1), and two other interface connects liquid phase color respectively Compose column outlet and derivative liquid entrance；The other end of derivatization reaction pipe (1) is connected to fluorescence detector；Temperature sensor (8) is fixed On the riser of lower cover (7)；The upper cover plate (9) is fixed together by screw and samming body (5), and is fastened on derivative Reaction tube (1), heat conducting pipe (2), the top of samming body (5) and mixing tee (4)；Upper cover plate (9) and lower cover (7) form closed Cuboid samming inner chamber, as derivatization device core；The outside of derivatization device core is provided with heat-preservation cotton (10), is placed in lagging casing (11) In.
- 2. derivatization device according to claim 1, it is characterised in that：The material of the derivatization reaction pipe (1) is polytetrafluoroethyl-ne Alkene (PTFE) or fluorinated ethylene propylene copolymer (FEP), pipe range 7-12m, external diameter 1.0-1.6mm, internal diameter 0.3-0.5mm, pipe Both ends intubating length 8-10mm stainless steel tube (101), the internal diameter of the external diameter and derivatization reaction pipe (1) of stainless steel tube (101) are fitted Match somebody with somebody, internal diameter 0.2-0.3mm.
- 3. derivatization device according to claim 1, it is characterised in that：The heat conducting pipe (2) is long 60-110mm, external diameter 6- 11mm, internal diameter 3-5mm metal straight pipe.
- 4. derivatization device according to claim 1, it is characterised in that：The mixing tee (4) is the general mark of liquid chromatogram Quasi- three-way connector.
- 5. derivatization device according to claim 1, it is characterised in that：The heat conducting pipe (2), samming body (5), lower cover (7) Material with upper cover plate (9) is heat conductivility good metallic aluminium, copper or stainless steel.
- 6. derivatization device according to claim 1, it is characterised in that：The material of the heat-preservation cotton (9) is with relatively low heat conduction Melamine foamed plastic, glass fibre cotton or the ceramic fiber cotton of coefficient.
- 7. derivatization device according to claim 1, it is characterised in that：Between the samming body (5) and lower cover (7), add One layer of uniform heat-conducting silicone grease is coated between hot core (6) and samming body (5) and between mixing tee (4) and samming body (5) simultaneously Closely amplexiform.
- 8. derivatization device according to claim 1, it is characterised in that：The samming body (5) is block, and heating core (6) is Electrically heated rod.
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| CN201610848268.XA CN107870219B (en) | 2016-09-26 | 2016-09-26 | Small chemical derivatization device |
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| CN107870219B (en) | 2020-09-01 |
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