JPH0698303B2 - Micro reaction and preparative equipment - Google Patents

Micro reaction and preparative equipment

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Publication number
JPH0698303B2
JPH0698303B2 JP60087633A JP8763385A JPH0698303B2 JP H0698303 B2 JPH0698303 B2 JP H0698303B2 JP 60087633 A JP60087633 A JP 60087633A JP 8763385 A JP8763385 A JP 8763385A JP H0698303 B2 JPH0698303 B2 JP H0698303B2
Authority
JP
Japan
Prior art keywords
capillary tube
reaction
valve
preparative
liquid chromatograph
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
JP60087633A
Other languages
Japanese (ja)
Other versions
JPS61245837A (en
Inventor
善明 西原
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Sumitomo Heavy Industries Ltd
Original Assignee
Sumitomo Heavy Industries Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Sumitomo Heavy Industries Ltd filed Critical Sumitomo Heavy Industries Ltd
Priority to JP60087633A priority Critical patent/JPH0698303B2/en
Publication of JPS61245837A publication Critical patent/JPS61245837A/en
Publication of JPH0698303B2 publication Critical patent/JPH0698303B2/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0093—Microreactors, e.g. miniaturised or microfabricated reactors
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/24—Stationary reactors without moving elements inside
    • B01J19/2415—Tubular reactors
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/24—Stationary reactors without moving elements inside
    • B01J19/2415—Tubular reactors
    • B01J19/243—Tubular reactors spirally, concentrically or zigzag wound
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
    • B01J2219/00076—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements inside the reactor
    • B01J2219/00081—Tubes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
    • B01J2219/00105—Controlling the temperature by indirect heating or cooling employing heat exchange fluids part or all of the reactants being heated or cooled outside the reactor while recycling
    • B01J2219/00108—Controlling the temperature by indirect heating or cooling employing heat exchange fluids part or all of the reactants being heated or cooled outside the reactor while recycling involving reactant vapours
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B01J2219/0015—Controlling the temperature by thermal insulation means
    • B01J2219/00155—Controlling the temperature by thermal insulation means using insulating materials or refractories
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/00788—Three-dimensional assemblies, i.e. the reactor comprising a form other than a stack of plates

Description

【発明の詳細な説明】 産業上の利用分野 本発明は生体物質、天然物等の微量物質の合成に用いら
れる自動ミクロ反応装置に関し、また特に微量かつ純度
の要求される放射性同位元素標識薬剤等を合成し、直ち
に得られた反応生成物を分離し得るミクロ反応及び分取
装置に関する。TECHNICAL FIELD The present invention relates to an automatic microreactor used for the synthesis of trace substances such as biological substances and natural products, and more particularly to radioisotope-labeled drugs which require trace amounts and purity. The present invention relates to a microreaction and a preparative device capable of synthesizing a compound and immediately separating a reaction product obtained.

従来の技術 従来、微量物質の合成、例えばトレーサーとして用いら
れる医療用の放射性同位元素を用いた薬剤の合成は、適
宜の薬剤中間体に、前駆物質である例えば、11CH3Iを反
応させて製造（例えば、N-メチル‐スピペロン等）され
るが、従来の装置では、まず低温（例えば‐20℃以下）
に保持された反応器内の有機溶媒液中に、キャリアガス
をバブリングし、このキャリアガス中に含まれる11CH3I
（メチル化剤）を前記有機溶媒にトラップさせる。その
後、該11CH3I含有有機溶媒に、薬剤中間体を加えて、数
分間加熱（40〜80℃）して反応させることにより、前記
標識薬剤を製造していた。そして、更にこの薬剤は、分
取用液体クロマトグラフ装置に導入して分取されてい
た。2. Description of the Related Art Conventionally, the synthesis of a trace substance, for example, the synthesis of a drug using a medical radioisotope used as a tracer, involves reacting an appropriate drug intermediate with a precursor such as 11 CH 3 I. It is manufactured (for example, N-methyl-spiperone, etc.), but in the conventional equipment, it is first at low temperature (for example, below -20 ° C)
A carrier gas was bubbled into the organic solvent liquid in the reactor held in the chamber, and 11 CH 3 I contained in the carrier gas was bubbled.
(Methylating agent) is trapped in the organic solvent. Then, the labeled drug was manufactured by adding a drug intermediate to the 11 CH 3 I-containing organic solvent and heating (40 to 80 ° C.) for several minutes to react. Further, this drug has been introduced into a preparative liquid chromatograph apparatus for fractionation.

発明が解決しようとする問題点 しかしながら、そうした装置では、反応器から反応生成
物を取り出し、その後これを分取用クロマトグラフにか
けるのであるが、それはほとんど手操作で行われるため
に、反応から分取までに要する時間が長く、特に半減期
の短い放射性同位元素薬剤を合成する場合に非常に不利
となる。DISCLOSURE OF THE INVENTION Problems to be Solved by the Invention However, in such an apparatus, the reaction product is taken out of the reactor and then subjected to preparative chromatograph, which is separated from the reaction because it is almost manually performed. It takes a long time to collect, which is extremely disadvantageous especially when synthesizing a radioisotope drug having a short half-life.

また従来の装置では、放射性同位元素薬剤を取り扱う場
合でも、オンラインによる合成及び分離が行われる構造
となっていないため、そのハンドリング時における被曝
の危険性があった。Further, in the conventional device, even when handling a radioisotope drug, there is a risk of exposure during handling because the structure does not allow online synthesis and separation.

更に従来の装置では、分取用の特別のカラムを必要とす
るため、余分な機器、スペースを必要とし、経済的にも
不利であるという、いくつかの問題点を有していた。Further, the conventional apparatus has some problems that it requires a special column for fractionation, which requires extra equipment and space and is economically disadvantageous.

そして、前述のごとき特別の目的に供される薬剤等の合
成においては、非常にミクロな反応系（微量物質の反応
系）が要求されるところ、従来装置では微少量の薬剤同
士の反応を効率的に行うことはできなかった。In the synthesis of drugs that serve special purposes such as those mentioned above, a very micro reaction system (reaction system for trace substances) is required. I couldn't do it.

問題点を解決するための手段 本発明者は、上記の問題点を解決するために鋭意研究し
た結果、液体クロマトグラフのインジェクション部にお
ける分取用ループ（キャピラリーチューブ）を反応帯域
として応用することを着想した。Means for Solving the Problems As a result of earnest research for solving the above problems, the present inventor has found that a preparative loop (capillary tube) in an injection part of a liquid chromatograph is applied as a reaction zone. I got the idea.

したがって、本発明は、このような着想に基づいて発明
されたものであって、熱供給部と冷媒供給部を備えた保
温容器内にキャピラリーチューブを曲折して設けてなる
反応器と液体クロマトグラフ装置ならびに試料供給管と
を６方バルブからなるサンプルインジェクタを介して接
続して構成したことを特徴とするミクロ反応及び分取装
置を構成要件とするものである。Therefore, the present invention was invented based on such an idea, and a reactor and a liquid chromatograph provided by bending a capillary tube in a heat-retaining container having a heat supply section and a refrigerant supply section. The microreaction and fractionation device is characterized in that the device and the sample supply pipe are connected via a sample injector consisting of a 6-way valve.

前記キャピラリーチューブは、この中の管壁に前駆物質
をトラップし、反応帯域となる場所であると共に、液体
クロマトグラフを使用した分取時には、サンプルインジ
ェクターに付属しているループの役割を果たすもので、
テフロン、ガラス、金属（特にステンレス等）などの細
管で構成されるが、高速液体クロマトグラフを用いる場
合は、高圧に耐えられる材料が良く、ステンレス管が好
ましい。The capillary tube is a place where the precursor is trapped in the wall of the capillary tube and serves as a reaction zone, and also serves as a loop attached to the sample injector at the time of fractionation using a liquid chromatograph. ,
It is composed of a thin tube such as Teflon, glass, metal (in particular, stainless steel, etc.), but when using a high performance liquid chromatograph, a material capable of withstanding high pressure is preferable and a stainless tube is preferable.

キャピラリーチューブの内径は、0.5mm以下のものが用
いられ、長さは100mmのものが用いられるが、これに限
定されるものではない。The inner diameter of the capillary tube is 0.5 mm or less and the length is 100 mm, but the inner diameter is not limited to this.

また、キャピラリーチューブは、ら旋状、コイル状、渦
巻き状などの所望の形状に巻いて用いることができ、そ
うしたものを使用することにより、それを収容する反応
器を非常に小型化することができるのである。Further, the capillary tube can be used by winding it into a desired shape such as a spiral shape, a coil shape, or a spiral shape, and by using such a shape, the reactor for accommodating it can be extremely miniaturized. You can do it.

次に、キャピラリーチューブを収納する保温容器は、反
応帯域を加熱したり又は冷却したりする必要があり、そ
の温度保持が目的であるので、断熱材からなるか又は断
熱材の充填された容器が用いられる。該容器は、円筒
状、方形状など適宜の形状にすることができる。断熱材
としては、コルク、綿、フェルト、発泡スチロール、ア
スベスト、ガラスウール等が用いられ、これらの材料
は、使用温度にしたがって適宜選択する。また真空によ
る断熱効果（例えば、魔法びん）を利用したものを用い
ても良い。保温容器の底部には、熱風などの熱供給部と
液体炭酸ガス、液体窒素などの冷媒供給部が配設されて
いる。Next, the heat-retaining container that stores the capillary tube needs to heat or cool the reaction zone, and since the purpose is to maintain the temperature, a container made of a heat insulating material or a container filled with a heat insulating material should be used. Used. The container can have any suitable shape such as a cylindrical shape or a rectangular shape. As the heat insulating material, cork, cotton, felt, styrofoam, asbestos, glass wool, etc. are used, and these materials are appropriately selected according to the operating temperature. Moreover, you may use what used the heat insulation effect by vacuum (for example, a thermos bottle). A heat supply unit such as hot air and a coolant supply unit such as liquid carbon dioxide gas and liquid nitrogen are arranged at the bottom of the heat insulating container.

熱供給部は、例えば加熱用ノズルで構成され、また冷媒
供給部は、冷却用ノズルで構成されており、これから噴
出する熱風又は冷気の制御は、共に電磁弁又は手動コッ
クなどにより行なわれる。The heat supply unit is composed of, for example, a heating nozzle, and the refrigerant supply unit is composed of a cooling nozzle. Both hot air and cold air ejected from the refrigerant supply unit are controlled by a solenoid valve or a manual cock.

また保温容器の底面に熱電素子を用いたサーモモジュー
ルを設けることも可能であり、更に冷却においては、こ
れと上記液体炭酸ガス、液体窒素、液体空気などの冷却
媒体と組み合わせて用いてもよい。温度センサーとして
は、温度計、熱電対温度計などが用いられる。It is also possible to provide a thermomodule using a thermoelectric element on the bottom surface of the heat insulating container, and in cooling, this may be used in combination with a cooling medium such as the above liquid carbon dioxide gas, liquid nitrogen or liquid air. A thermometer, a thermocouple thermometer, etc. are used as a temperature sensor.

以上のごとき反応器を使用して、ミクロ反応が行なわれ
るが、まず、キャピラリーチューブには、有機溶剤が導
入される。しかしこれは、前駆物質のキャピラリーチュ
ーブへの付着を促進するための工程であるから、付着が
少なくてよい場合は、この工程は省略してもよい。A micro reaction is carried out using the reactor as described above, but first, an organic solvent is introduced into the capillary tube. However, since this is a step for promoting the adhesion of the precursor to the capillary tube, this step may be omitted if the adhesion may be small.

導入される有機溶媒としては、アセトン、ベンゼン、ト
ルエンTHF等が用いられ、これらの有機溶媒は、キャピ
ラリーチューブの内壁面に付着される。Acetone, benzene, toluene THF or the like is used as the introduced organic solvent, and these organic solvents are attached to the inner wall surface of the capillary tube.

次にキャリアガスを導入することにより、該キャリアガ
ス中に含有される前駆物質は前記キャピラリーチューブ
内壁面に付着した有機溶媒でトラップされる。トラップ
効率を上げるためには、反応帯域を冷却（例えば−20〜
−60℃）するのがよい。Then, by introducing a carrier gas, the precursor contained in the carrier gas is trapped by the organic solvent attached to the inner wall surface of the capillary tube. To increase the trap efficiency, cool the reaction zone (for example, -20 ~
-60 ℃) is recommended.

なお、キャリアガスとしては、窒素、空気又はヘリウ
ム、アルゴンなどの不活性気体が用いられる。As the carrier gas, nitrogen, air, or an inert gas such as helium or argon is used.

このようにしてキャピラリーチューブには、前駆物質を
トラップした後、該キャピラリーチューブへ薬剤（液体
状のもの又は溶媒に溶かしたものあるいは霧状のものな
ど）を導入して前駆物質と反応させる。In this manner, after the precursor is trapped in the capillary tube, a drug (liquid, dissolved in a solvent, atomized, or the like) is introduced into the capillary tube to react with the precursor.

反応温度は反応物質の種類により異なるが、11CH3Iなど
の前駆物質を用いた場合、約40〜80℃の温度に反応帯域
を保持して行うのが好ましい。反応が完結した後、該生
成物をサンプルインジェクター操作し、これを通して液
体クロマトグラフ装置へ導入し、所望の生成物を分取す
る。The reaction temperature varies depending on the kind of the reaction substance, but when a precursor such as 11 CH 3 I is used, it is preferable to carry out the reaction while maintaining the reaction zone at a temperature of about 40-80 ° C. After the reaction is completed, the product is operated by a sample injector, and is introduced into a liquid chromatograph through the sample injector to separate a desired product.

そして分取時には、サンプルインジェクターに接続され
ている試料供給管のバルブは生成物の逆流を防止するた
めに閉鎖しておく。At the time of collection, the valve of the sample supply pipe connected to the sample injector is closed to prevent the product from flowing backward.

サンプルインジェクターは、液体クロマトグラフに用い
られているものであり、６方バルブを有するサンプルイ
ンジェクターであって、その端部には、液体クロマトグ
ラフ装置のポンプ、液体クロマトグラフ装置のカラム、
ベントなどが接続され、更に反応器のキャピラリーチュ
ーブの両端が接続される。The sample injector is used in a liquid chromatograph and is a sample injector having a 6-way valve, and a pump of the liquid chromatograph device, a column of the liquid chromatograph device,
A vent or the like is connected, and further both ends of the capillary tube of the reactor are connected.

なおキャピラリーチューブの一方には、バルブを有する
試料供給管が分岐している。A sample supply pipe having a valve is branched to one of the capillary tubes.

液体クロマトグラフとしては、吸着クロマトグラフ、分
配クロマトグラフ、高速液体クロマトグラフなどの装置
が使用される。As the liquid chromatograph, a device such as an adsorption chromatograph, a partition chromatograph, a high performance liquid chromatograph is used.

実施例 本発明の実施例を第１図及び第２図をもって説明する。Embodiment An embodiment of the present invention will be described with reference to FIGS. 1 and 2.

第１図は本発明の反応時のサンプルインジェクターの連
続関係を示す説明図であつて、１はサンプルインジェク
ターであり、六方バルブを有するものである。バルブ番
号Ｉ及びIVにはキャピラリーチューブの両端が接続され
ており、バルブ番号IVに接続されたキャピラリーチュー
ブの端部には、バルブ７を有する試料供給管が合流して
いる。試料供給管からは、有機溶媒あるいは前駆物質及
び反応薬剤中間体をキャピラリーチューブ２へ供給す
る。バルブ番号IIには、液体クロマトグラフ装置のポン
プが接続される。反応生成物の分取時には第２図に示さ
れているごとく、バルブ番号Ｉとバルブ番号IIとが接続
されて、溶離液が供給される。バルブ番号IIIには、液
体クロマトグラフ装置のカラムが接続されており、バル
ブ７が閉鎖されると共にバルブ番号IIIとバルブ番号IV
とが接続されて、反応生成物がカラムへ移送される。な
お、バルブ番号VIはベントに接続されている。FIG. 1 is an explanatory view showing the continuous relationship of sample injectors during the reaction of the present invention, in which 1 is a sample injector, which has a hexagonal valve. Both ends of the capillary tube are connected to the valve numbers I and IV, and the sample supply pipe having the valve 7 is joined to the end of the capillary tube connected to the valve number IV. From the sample supply pipe, the organic solvent or precursor and the reactive drug intermediate are supplied to the capillary tube 2. A pump of the liquid chromatograph device is connected to the valve number II. At the time of collecting the reaction product, as shown in FIG. 2, the valve number I and the valve number II are connected and the eluent is supplied. The column of the liquid chromatograph is connected to the valve number III, and the valve 7 is closed and the valve number III and the valve number IV are connected.
Are connected to transfer the reaction product to the column. The valve number VI is connected to the vent.

３は断熱材からなる容器であり該容器には、その底面に
加熱用ノズル４及び冷却用ノズル５が設けられており、
更に側壁には熱電対温度計６が設置されている。そして
該容器内には、内径0.5mm、長さ1000mmのコイル状に形
成されたキャピラリーチューブ２が収納されている。3 is a container made of a heat insulating material, which is provided with a heating nozzle 4 and a cooling nozzle 5 on its bottom surface,
Further, a thermocouple thermometer 6 is installed on the side wall. A coiled capillary tube 2 having an inner diameter of 0.5 mm and a length of 1000 mm is housed in the container.

まず、第１図に示されているように、反応時にはキャピ
ラリーチューブは反応器の役割を果たす。サンプルイン
ジェクター１においてバルブ番号Ｉとバルブ番号VIが、
バルブ番号IIとバルブ番号IIIとが、それぞれ接続する
ようにセットし、バルブ７を開放して、キャピラリーチ
ューブ２へアセトンを導入すると、アセトンはキャピラ
リーチューブ２の内壁面に付着した。First, as shown in FIG. 1, the capillary tube plays the role of a reactor during the reaction. In sample injector 1, valve number I and valve number VI are
When the valve numbers II and III were set so as to be connected to each other, the valve 7 was opened, and acetone was introduced into the capillary tube 2, the acetone adhered to the inner wall surface of the capillary tube 2.

次に冷却用ノズル５から液体炭酸ガスを噴出せしめ、キ
ャピラリーチューブ２を−20〜−60℃に冷却し、この冷
却下に窒素からなるキャリアガスに混合した11CH3Iをキ
ャピラリーチューブ２内を通し、該キャリアガスに含ま
れている11CH3Iをキャピラリーチューブ２内壁面のアセ
トンに捕そくさせた。その後、スピペロンのトルエン溶
液をキャピラリーチューブ２内へ導入した後、保温容器
３へ熱風を吹き込んで、約50℃に維持して反応を進行さ
せた。Next, liquid carbon dioxide gas was ejected from the cooling nozzle 5, the capillary tube 2 was cooled to −20 to −60 ° C., and under this cooling, 11 CH 3 I mixed with a carrier gas consisting of nitrogen was charged into the capillary tube 2. 11 CH 3 I contained in the carrier gas was trapped in acetone on the inner wall surface of the capillary tube 2. After that, a toluene solution of spiperone was introduced into the capillary tube 2, and then hot air was blown into the heat insulating container 3 to maintain the temperature at about 50 ° C. to allow the reaction to proceed.

反応が完了した後、第２図に示されているように、サン
プルインジェクター１を時計方向に約60゜回転させ、バ
ルブ番号Ｉとバルブ番号II及びバルブ番号IIIとバルブ
番号IVとをそれぞれ接続し、バルブ７を閉鎖してから液
体クロマトグラフのポンプを始動させて、キャピラリー
チューブ２内の反応生成物を液体クロマトグラフ装置の
カラムへ導入した。After the reaction was completed, as shown in FIG. 2, the sample injector 1 was rotated clockwise about 60 ° to connect the valve numbers I and II and the valve numbers III and IV, respectively. After closing the valve 7, the pump of the liquid chromatograph was started to introduce the reaction product in the capillary tube 2 into the column of the liquid chromatograph.

該カラムを通過して分取された反応生成物は、11C−Ｎ
−メチルスピペロンの構造式の放射性同位元素標識薬剤
であった。The reaction product separated through the column was 11 C-N
It was a radioisotope-labeled drug with the structural formula of methylspiperone.

発明の効果 以上のとおり、本発明は曲折したキャピラリーチューブ
によって反応器を構成したので、従来装置のようなバブ
リングによる反応装置とは異なり、小型化装置内でのミ
クロ合成が可能となり、また反応時間を短縮することも
できた。As described above, according to the present invention, since the reactor is constituted by the bent capillary tube, it is possible to perform micro-synthesis in the miniaturization device and to reduce the reaction time unlike the reaction device by bubbling like the conventional device. Could also be shortened.

そして、反応部と分取部を一体化して、オンラインによ
る合成、分取が可能となり、放射性反応物を対象とする
場合に、被曝の危険性がなくなった。And, by integrating the reaction part and the preparative part, it is possible to perform online synthesis and preparative work, and there is no risk of radiation exposure when targeting radioactive reactants.

更には、反応生成物が微量であるため、従来常用の分析
用カラムをそのまま使用することができ、分取用の特別
のカラムを使用する必要がなくなつたなど、従来に例の
ない格別の優れた作用効果を奏するものである。Furthermore, since the reaction product is in a trace amount, the conventional analytical column can be used as it is, and it is no longer necessary to use a special column for fractionation. It has excellent effects.

【図面の簡単な説明】[Brief description of drawings]

第１図は、本発明実施例のミクロ反応装置（反応時）の
説明図であり、第２図は同反応装置の分取時のサンプル
インジェクターの接続関係を示した説明図である。 1:サンプルインジェクター 2:キャピラリーチューブ（反応器） 3:断熱材（容器） 4:加熱用ノズル 5:冷却用ノズル 6:温度センサー 7:バルブFIG. 1 is an explanatory diagram of a micro reactor (during reaction) of an example of the present invention, and FIG. 2 is an explanatory diagram showing a connection relationship of sample injectors during fractionation of the reactor. 1: Sample injector 2: Capillary tube (reactor) 3: Heat insulating material (vessel) 4: Nozzle for heating 5: Nozzle for cooling 6: Temperature sensor 7: Valve

Claims (2)

【特許請求の範囲】[Claims] 【請求項１】熱供給部と冷媒供給部を備えた保温容器内
にキャピラリーチューブを曲折して設けてなる反応器と
液体クロマトグラフ装置ならびに試料供給管とを６方バ
ルブからなるサンプルインジェクタを介して接続して構
成したことを特徴とするミクロ反応及び分取装置。1. A reactor provided by bending a capillary tube in a heat-retaining container having a heat supply section and a refrigerant supply section, a liquid chromatograph apparatus, and a sample supply tube via a sample injector consisting of a six-way valve. A micro-reaction and preparative device characterized by being connected and connected. 【請求項２】特許請求の範囲第（１）項記載のミクロ反
応及び分取装置を放射性同位元素化合物合成用に使用し
たことを特徴とするミクロ反応及び分取装置。2. A microreaction and preparative apparatus, characterized in that the microreaction and preparative apparatus according to claim 1 is used for synthesizing a radioisotope compound.
JP60087633A 1985-04-25 1985-04-25 Micro reaction and preparative equipment Expired - Lifetime JPH0698303B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP60087633A JPH0698303B2 (en) 1985-04-25 1985-04-25 Micro reaction and preparative equipment

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP60087633A JPH0698303B2 (en) 1985-04-25 1985-04-25 Micro reaction and preparative equipment

Publications (2)

Publication Number Publication Date
JPS61245837A JPS61245837A (en) 1986-11-01
JPH0698303B2 true JPH0698303B2 (en) 1994-12-07

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ID=13920377

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Country Link
JP (1) JPH0698303B2 (en)

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US6605475B1 (en) * 1999-04-16 2003-08-12 Perspective Biosystems, Inc. Apparatus and method for sample delivery
GB0206117D0 (en) * 2002-03-15 2002-04-24 Imaging Res Solutions Ltd Use of microfabricated devices
JP4920301B2 (en) * 2006-05-10 2012-04-18 住友重機械工業株式会社 RI compound synthesis apparatus and RI compound synthesis method
WO2008128201A1 (en) * 2007-04-12 2008-10-23 Siemens Medical Solutions Usa, Inc. Microfluidic radiosynthesis system for positron emission tomography biomarkers
DE102009014626A1 (en) * 2009-03-24 2010-10-07 Oxea Deutschland Gmbh Process for the preparation of aliphatic carboxylic acids from aldehydes by microreaction technology
JP6164880B2 (en) * 2013-03-11 2017-07-19 日本メジフィジックス株式会社 An instrument that provides a temperature control unit that is easy to assemble

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US4299498A (en) * 1979-12-03 1981-11-10 E. I. Du Pont De Nemours And Company Flashing reactor
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