CN101104627A - 18F-FDG automatization synthetic method and device - Google Patents
18F-FDG automatization synthetic method and device Download PDFInfo
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- CN101104627A CN101104627A CNA2007101299129A CN200710129912A CN101104627A CN 101104627 A CN101104627 A CN 101104627A CN A2007101299129 A CNA2007101299129 A CN A2007101299129A CN 200710129912 A CN200710129912 A CN 200710129912A CN 101104627 A CN101104627 A CN 101104627A
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Abstract
Disclosed is an 18F-FDG automatic synthesis method and equipment, relating to prepare the 18F-FDG through a nucleophilic reaction. In the invention, a vessel for reaction solution is communicated with a reaction vessel through a valve and a pipe. Under the control of a stepping motor, the reaction solution can be put into the reaction vessel in batch according to the need. The reaction vessel is communicated with plurality sets of product collecting devices through the pipe and a valve with one inlet and a plurality of outlets with which the product in the reaction vessel can be moved into the collecting devices. With the above-mentioned method, when the nucleophilic reaction is processed and the sealed reaction vessel is between 100 DEG C to 120 DEG C, the water removal and the nucleophilic reaction can be processed in one heating device. The equipment can realize one time charge and multiple synthesis. The method simplifies the heating device. The invention is mainly used in one-time charge and batch production of the radiopharmaceuticals.
Description
Technical field
The present invention relates to a kind of positron emission tomography (PET) (PET) diagnosis used radiopharmaceuticals 2-fluoro-18 generation-2 deoxidation-β-D-glucose (
18F-FDG) automatic synthesis method and equipment relate in particular to by nucleophilic reaction and prepare
18The method and apparatus of F-FDG.
Background technology
18F-FDG is widely used in the glucose metabolism mensuration etc. of diagnosis, cardiac muscle and the brain of malignant tumour.At present, widely used in the world
18The F-FDG synthetic method is based on the three-dimensional nucleophilic reaction principle of selectivity of Hamacher K in 1986 report, synthesizes β-D-2-fluorodeoxyglucose.Along with clinical right
18The demand of F-FDG is increasing, and the researchist has mainly carried out research from two aspects: (1) improves single synthetic efficient.High efficiency synthesizing of single not only improved
18The output of F-FDG has also been saved production simultaneously
18The cost of F-FDG.But because
18The transformation period of F only is 110 minutes, if synthesize 96mCi's morning
18F-FDG, use in 6 hours decay to 12mCi, then is 6mCi after 8 hours.Clearly, single synthetic amount is not only wasted greatly, and is difficult to satisfy clinical long-time demand.Therefore, more domestic hospitals or company have been equipped with many
18The F-FDG synthesizer is so that produce in batches as required.Be equipped with many platform independent
18The F-FDG synthesizer has improved production cost greatly.And, because
18F-FDG is synthetic to carry out under the radioactivity condition, and relevant device need place under the lead protection of 60mm, and promptly every cover synthesis device all has an independently synthetic protective housing, thereby its production cost is enhanced again.And the idle meeting of multiple devices causes great waste.(2) the repeatedly synthetic technology under the same module of exploitation, the once charging under the promptly same synthesizer, repeatedly synthetic.As twice synthetic technology of Black-to-Black of CTI company (Bruce H.Mock, Michael T.:Back-to-back " one-pot " [
18F] FDG syntheses in a singleSiemens-CTI chemistry process control unitNuclear Medicine andBiology, Volume 23, Issue 4, May 1996, Pages 497-501) and the dual system of GE company
18(General Electric (China) medical system portion, the FDG of GE a new generation chemistry is synthesis system automatically for the F-FDG synthetic technology.World medicine equipment 200,1V7,N12 68), all are two synthesis systems that adopt in the same synthesizer, have two to overlap independently synthesis system in the promptly same synthesizer, two cover reaction tubess, two cover reagent.The advantage of this system is that permission secondary under active situation is synthetic.But this system can not surpass secondary, therefore, is only applicable to part hospital, and is right
18Bigger hospital or the company of F-FDG amount still can not satisfy the demand.Therefore be necessary to develop a kind of can on a synthesizer, repeatedly synthesizing
18The novel method of F-FDG and equipment when satisfying production, are minimized cost.And have the operation that reaction soln is moved into reaction vessel now, what generally adopt is pneumatic/negative pressure mode, still can't realize the controlled of reaction soln pipetted.
In addition, as previously mentioned, existing synthetic method all is to utilize the nucleophilic reaction principle, and the process need of this reaction dewaters by heating, and then finishes nucleophilic reaction under heating condition.But must be owing to dewater more than 100 ℃, and the boiling point that reacts required reagent acetonitrile is 81 ℃, intermediate product
18The boiling point of FDG is 82 ℃, so this different Heating temperature proposes higher requirement to heating unit.
Summary of the invention
The object of the present invention is to provide and a kind ofly can satisfy the production needs, the repeatedly automatization that can reduce production costs greatly again
18F-FDG synthetic method and equipment.
First purpose of the present invention is achieved by the following technical solution:
A kind of
18The automatic synthesis method of F-FDG comprises the steps:
(1) adopts the K2.2.2 acetonitrile solution wash-out that contains salt of wormwood
18F-boils elute soln to doing under 100～120 ℃ of temperature;
(2) cooling adds the mannose triflate anhydrous acetonitrile;
(3) in confined conditions, will contain
18The mannose triflate anhydrous acetonitrile heating of F-finishes up to nucleophilic reaction;
(4) cooling, collecting reaction product, and be hydrolyzed, wash-out and purification process;
Wherein: the adding of reaction soln is carried out as required in batches in step (1), (2); Accordingly, the collection of reaction product in the step (4), and hydrolysis, wash-out and purification process are also carried out in batches; And also be included in the operation of with anhydrous acetonitrile and water reaction vessel being cleaned between each reaction batch.
Automatization synthesis device of the present invention, comprise the container, reaction vessel, heating unit, the product collection device that hold reaction soln/water, wherein, the container that holds reaction soln communicates with reaction vessel by pipeline and valve respectively, and is provided with the QMA post on container that holds the K2.2.2 acetonitrile solution that contains salt of wormwood and the pipeline between the reaction vessel; Reaction vessel communicates with the product collection device by corresponding pipeline and valve, and this pipeline stretches into the bottom in reaction vessel, and this pipeline also communicates with the device that holds nitrogen by valve; Reaction vessel also communicates with air and/or nitrogen by another pipeline and respective valves, and this pipeline stretches into the top of reaction vessel in reaction vessel; Heating unit is positioned at the reaction vessel bottom; Wherein: the container that holds reaction soln all links to each other with stepper-motor; On the pipeline between reaction vessel and the collection device, be provided with one and advance to have more valve, and the product collection device also there are corresponding many covers near an end of collection device.
Utilize method and apparatus of the present invention, corresponding reaction soln can be under step motor control, being moved in the same reaction vessel in batches of amount as required reacted, generating desired product, and advance to have more valve and corresponding many cover collection devices are collected product by one in that device is terminal.Thereby can accomplish once to feed, synthetic in batches, promptly begin in the container that holds reaction soln/water, to add enough solution, then, in reaction vessel, move into the solution of aequum as required earlier, after the reaction, advance to have more valve by one of collection device front end product is moved in the cover collection device of equipment end.With acetonitrile and water the reaction vessel automatization is cleaned up the back and wait for reaction next time.When treating to synthesize again, the reaction soln with aequum moves into reaction vessel again, after question response finishes, advances to have more valve by collection device front end one product is moved into the another set of collection device of wanting.
Because the present invention has accomplished to utilize a cover reaction unit, once charging, synthetic in batches, therefore, the present invention is right in solution
18In the time of this problem of F-FDG demand height, greatly reduce cost, reduced that spatial is taken.And, when carrying out nucleophilic reaction, can be easy to the airtight of realization response container, reaction is carried out in confined conditions, avoid reaction soln acetonitrile and intermediate
18FDG-(Ac) 4 explosive evaporatoins, and temperature of reaction also can be 100～120 ℃, the temperature that dewaters is identical with beginning to boil, and therefore, can finish with a cover simple heating device.
As the technical scheme that synthesis device of the present invention is further limited, hold on the container of reaction soln and the pipeline between the reaction vessel at each and to be equipped with the intermediate transfer container, and the intermediate reaction container all links to each other with the device that holds nitrogen.Like this, can be at first the reaction soln of every batch of aequum be moved into corresponding transfer container by stepper-motor, then, with nitrogen the solution in the transfer container is pressed in the reaction vessel again, the liquid of having guaranteed each adding can all be transferred in the reaction vessel, reduced the residual waste that cause of reaction soln on transfer line, reduced the influence of the residual liquid on the transfer line simultaneously nucleophilic reaction.
Heating unit in the synthesis device of the present invention is positioned at the reaction vessel below, is made up of motor and electrically heated piece moving up and down; The corresponding position of electrically heated piece top and reaction vessel is provided with reaction vessel size and shape and slots accordingly.
The electrically heated piece is heated to temperature required in advance, when needing, only need that it is risen to the reaction vessel below and get final product, thereby the rapid realization of assurance heating reduces to heat required time, enhances productivity.Its notching construction has guaranteed simultaneously reaction vessel to be heated from a plurality of angles, equally also can reduce heat-up time, enhance productivity.Especially, this fixation reaction container moves up and down the setting of heating unit, sealing to reaction vessel is become realize easily.
Description of drawings
Accompanying drawing 1 is the composition synoptic diagram of an embodiment of present device.
Among the figure, 1,2, rolling bottle among the 3-, 4-holds the container of the K2.2.2 acetonitrile solution that contains salt of wormwood, 5-holds the container of anhydrous acetonitrile, and 6-holds the container of mannose triflate anhydrous acetonitrile, the 7-syringe, 8-holds the container of water, 9-reaction vessel, 10-electrically heated piece, 11-motor, 12-hold the syringe of NaOH, and 13-one advances six and goes out valve, the 14-collection device, 15-refrigerating unit, 16-the one C-18 post, the 17-IC-H post, 18-Al
2O
3Post, 19-the 2nd C-18 post, 20-receiving flask, 21-waste liquid bottle, 22-nitrogen, 23-variable valve, 24-check valve, 25-QMA post, 26-magnetic resonance acceleator; V0～V11-valve.
Below in conjunction with the drawings and specific embodiments the present invention is done to describe more specifically.
Embodiment
A kind of
18The automatization synthesis device of F-FDG, as shown in drawings.Wherein, the container 4 that holds K2.2.2 solution is connected with middle rolling bottle 1, and the container 5 that holds anhydrous acetonitrile is connected with middle rolling bottle 2, and the container 6 that holds the mannose triflate anhydrous acetonitrile is connected with middle rolling bottle 3.Hold the container 4 of the K2.2.2 acetonitrile solution that contains salt of wormwood, the container 6 that holds the container 5 of anhydrous acetonitrile and hold the mannose triflate anhydrous acetonitrile is commonly referred to as the container that holds reaction soln.In rolling bottle 1,2,3 advance one by two six-way valve V0 and three respectively and go out valve V1, V2, V3 and corresponding pipeline and be connected with reaction vessel 9, and all link to each other with the device that holds nitrogen.Entrance end of valve V0 communicates with magnetic resonance acceleator 26 outlets, can make to come from magnetic resonance acceleator 26
18F passes through.On the pipeline between valve V0 and valve V1, be provided with a QMA post 25, be used to catch and come from magnetic resonance acceleator 26
18F.Syringe 7 and the container 8 that holds water all are connected with the import of T-valve V8, T-valve V8 is communicated with T-valve V7, in two other mouthful of T-valve V7 one is connected with reaction vessel 9 by two-way valve V5, and another mouthful then communicates with the import of T-valve V4.Another import of T-valve V4 is connected with the container 22 that holds nitrogen, and outlet is connected with the import of T-valve V9, enters at nitrogen on the pipeline of valve V4 and is provided with variable valve 23 and check valve 24.
T-valve V9 outlet is advanced six by one and is gone out valve 13 and six and overlap collection devices 14 and communicate.Every suit collection device comprises a C-18 post 16, T-valve V11, IC-H post 17, Al successively
2O
3Post 18, the 2nd C-18 post 19, aseptic filter membrane and receiving flask 20.
Reaction vessel 9 also is connected with two-port valve V6, T-valve V10 successively, and wherein two other mouthful of valve V10 communicates with nitrogen and atmosphere respectively.
Hold the container 4,5,6 of reaction soln, syringe 7, and hold on the syringe 12 of NaOH and be equipped with stepper-motor.Being contained in NaOH solution in the syringe 12 can be under Stepping Motor Control be moved on the C-18 post 16 of collection device 14 by T-valve V9 and carries out hydrolysis reaction, the water that is contained in the container 8 can pass through the syringe transfer, by controlled being transferred among the valve V7 of the stepper-motor on the syringe 7, be contained in reaction soln in the container 4,5,6 can under corresponding Stepping Motor Control, transfer to corresponding in the rolling bottle 1,2,3, and and then under the nitrogen effect, be moved in the reaction vessel 9 by corresponding valve.
Said heating unit is made up of an electrically heated piece 10 and motor 11, is positioned at the below of reaction vessel 9.Whole heating unit can move up and down under motor 11 controls.Electrically heated piece 10 crown center positions have groove, and this groove size and shape are corresponding with reaction vessel 9.To reaction vessel 9 heating the time, by motor 11 electrically heated piece 10 is promoted, reaction vessel is entered in its groove, so that reduce to heat the used time, improve resultant velocity.
Refrigerating unit 15 can be an any structure, as air cooling equipment, as long as can make the reaction vessel cooling as early as possible.
Below by the mode of giving an example to using present device production
18The concrete operations of F-FDG are described in detail.
(1). produce by magnetic resonance acceleator 26
18F is caught by QMA post 25 through valve V0 by the nitrogen carrier band;
(2). utilize stepper-motor that the acetonitrile solution that the 1.5ml in the container 4 contains the K2.2.2 of salt of wormwood is joined in the middle rolling bottle 1, open valve V0, V1, the K2.2.2 acetonitrile solution that will contain salt of wormwood with nitrogen therefrom extrudes in the rolling bottle 1, through valve V0, with what adsorb on the QMA post 25
18The drip washing of F ion gets off to enter reaction vessel 9;
(3). in reaction vessel 9, feed nitrogen through valve V4, V7, V5, and open valve V6, valve V10, make reaction vessel 9 and air communication; The electrically heated piece 10 that is heated in advance more than 100 ℃ is promoted near reaction vessel 9, and heating makes acetonitrile and water azeotropic to doing;
(4). utilize stepper-motor with in the rolling bottle 2 during the 2ml anhydrous acetonitrile is transferred in the container 5, open valve V2, anhydrous acetonitrile in the middle rolling bottle 2 is added in the reaction vessel 9, continue to be heated to interior 9 liquid evaporations of reaction vessel and finish with nitrogen;
(5). move down electrically heated piece 10, and by refrigerating unit 15 reactor vessel cooled 9, utilize stepper-motor with in the rolling bottle 3 during 1ml mannose triflate anhydrous acetonitrile is transferred in the container 6, open valve V3, the mannose triflate acetonitrile solution is transferred in the reaction vessel 9 with nitrogen; Shut-off valve V6, and make valve V5 be in closing condition, thus with reaction vessel 9 sealings,, carry out nucleophilic reaction with moving on the electrically heated piece 10 that is heated in advance more than 100 ℃;
(6). question response finishes, and the electrically heated piece is moved down, and reactor vessel cooled 9 is utilized stepper-motor to extract 30ml water in container 8 and transferred to the syringe 7;
(7). by valve V8, V7 and V5,10ml water in the syringe 7 is moved to reaction vessel 9, open valve V10, V6, with nitrogen with the mixed solution in the reaction vessel 9 by valve V5, V7, V4, V9 and one advance six go out valve 13 transfer to first the cover collection device a C-18 post on.At this moment, intermediate is attracted on the C-18 post, and waste liquid enters waste liquid bottle 21 by the outlet of valve V11;
(8). repeating step (7) operation, wash an above-mentioned C-18 post with 10ml water in the syringe 7;
(9). open fluid inlet, first another outlet of overlapping collection device valve V11 that valve V9 links to each other with syringe 12, utilize stepper-motor that the NaOH solution 1ml of 2mol/L in the syringe 12 is joined on the C-18 post of the first cover collection device, intermediate is hydrolyzed;
(10). with stepper-motor with last 10ml water in the syringe 7 by valve V8, V7, V4, V9, and one advance six and go out valve 13 and move on the first cover collection device the one C-18 post 16 IC-H post 17, the Al of the back of flowing through successively again
2O
3Post 18, the 2nd C-18 post 19 purifying.Finally, product
18F-FDG enters receiving flask 20 through aseptic filter membrane.
In the aforesaid operations, the Heating temperature in step (3), (5) is advisable at 100～120 ℃.
Utilize said apparatus and operation, prepare a collection of the finished product
18F-FDG, production process was less than 23 minutes, and combined coefficient is greater than 60% (unattenuated correction).
Aforesaid operations is promptly finished one batch synthesizing.Synthetic again if desired, only need intermediate at first is transferred on the C-18 post of the second cover collection device, all the other operations are identical, but in the gap of twice operation, need clean reaction vessel with acetonitrile and water.Under the enough situation of initial original solution, utilize the method and apparatus of above-mentioned embodiment can carry out altogether six batches synthetic.
According to principle of the present invention, once produce after the charging batch, collection device can be arranged to any amount as required, as long as with one to advance to have more valve corresponding,, can carry out three batches production as advancing three and go out valve and think that corresponding three overlap collection devices with one.
Claims (6)
1. one kind
18The F-FDG automatic synthesis method comprises the steps:
(1) adopts the K2.2.2 acetonitrile solution wash-out that contains salt of wormwood
18F
-, under 100～120 ℃ of temperature, boil elute soln to doing;
(2) cooling adds the mannose triflate anhydrous acetonitrile;
(3) in confined conditions, will contain
18F
-Mannose triflate anhydrous acetonitrile heating, finish up to nucleophilic reaction;
(4) cooling, collecting reaction product, and be hydrolyzed, wash-out and purification process;
It is characterized in that: the adding of reaction soln is carried out as required in batches in step (1), (2); Accordingly, the collection of reaction product in the step (4), and hydrolysis, wash-out and purification process are also carried out in batches; And also be included in the operation of with anhydrous acetonitrile and water reaction vessel being cleaned between each reaction batch.
2. as claimed in claim 1
18The F-FDG automatic synthesis method is characterized in that: the Heating temperature in the step (3) is 100～120 ℃.
3. one kind
18F-FDG automatization synthesis device, comprise the container, reaction vessel, heating unit, the product collection device that hold reaction soln, wherein, the container that holds reaction soln communicates with reaction vessel by pipeline and valve respectively, and is provided with the QMA post on container that holds the K2.2.2 acetonitrile solution that contains salt of wormwood and the pipeline between the reaction vessel; Reaction vessel communicates with the product collection device by corresponding pipeline and valve, and this pipeline stretches into the bottom in reaction vessel, and this pipeline also communicates with the device that holds nitrogen by valve; Reaction vessel also communicates with air and/or nitrogen by another pipeline and respective valves, and this pipeline stretches into the top of reaction vessel in reaction vessel; Heating unit is positioned at the reaction vessel bottom; It is characterized in that: the container that holds reaction soln all links to each other with stepper-motor; On the pipeline between reaction vessel and the collection device, be provided with one and advance to have more valve, and the product collection device also there are corresponding many covers near an end of collection device.
4. as claimed in claim 3
18F-FDG automatization synthesis device is characterized in that: hold on the container of reaction soln and the pipeline between the reaction vessel at each and be equipped with the intermediate transfer container.
5. described as claim 3 or 4
18F-FDG automatization synthesis device is characterized in that: said heating unit is made up of motor and electrically heated piece moving up and down; The corresponding position of electrically heated piece top and reaction vessel is provided with reaction vessel size and shape and slots accordingly.
6. described as claim 3 or 4
18F-FDG automatization synthesis device is characterized in that: it is terminal to advance to have more valve since one, and every cover collection device comprises a C-18 post, T-valve, IC-H post, Al successively
2O
3Post, the 2nd C-18 post, aseptic filter membrane and receiving flask.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007101299129A CN101104627A (en) | 2007-07-20 | 2007-07-20 | 18F-FDG automatization synthetic method and device |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007101299129A CN101104627A (en) | 2007-07-20 | 2007-07-20 | 18F-FDG automatization synthetic method and device |
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| CN101104627A true CN101104627A (en) | 2008-01-16 |
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| CNA2007101299129A Pending CN101104627A (en) | 2007-07-20 | 2007-07-20 | 18F-FDG automatization synthetic method and device |
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