JPS62209352A - Thin layered chromatography mass analyser - Google Patents

Thin layered chromatography mass analyser

Info

Publication number
JPS62209352A
JPS62209352A JP61052865A JP5286586A JPS62209352A JP S62209352 A JPS62209352 A JP S62209352A JP 61052865 A JP61052865 A JP 61052865A JP 5286586 A JP5286586 A JP 5286586A JP S62209352 A JPS62209352 A JP S62209352A
Authority
JP
Japan
Prior art keywords
thin layer
ion
tank
development
specimen
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.)
Pending
Application number
JP61052865A
Other languages
Japanese (ja)
Inventor
Hitoshi Hoshino
星野 均
Toshio Ishihara
石原 敏夫
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.)
NEC Corp
Original Assignee
NEC Corp
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 NEC Corp filed Critical NEC Corp
Priority to JP61052865A priority Critical patent/JPS62209352A/en
Publication of JPS62209352A publication Critical patent/JPS62209352A/en
Pending legal-status Critical Current

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  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
  • Electron Tubes For Measurement (AREA)

Abstract

PURPOSE:To simplify the operation of qualitative analysis and to detect a specimen with high sensitivity, by directly detecting the specimen on a thin layer after development in chromatography by the RF discharge device in a development tank to perform the separation of mass. CONSTITUTION:A specimen is placed on a thin layer 1 and fallen until the lower part of the thin layer 1 is immersed in the developing solvent 8 received in a developing tank 14 to perform the development of the specimen. After the finish of development, the solvent 8 is discharged out of the tank 14 to evacuate the tank 14. Voltage is applied to a hollow cathode 2 and an anode 4 and high frequency power is applied to a RF coil 3 to form RF plasma in the cathode 2. The surface of the thin layer 1 is sputtered by said plasma and the developed specimen is ionized. The ion is accelerated by the ion acceleration electrode 5 of an ion acceleration apparatus 21 to be incident to a Q-pole mass analyser 6 and the ion subjected to mass separation is detected by ion detector to perform qualitative analysis.

Description

【発明の詳細な説明】 [産業上の利用分野] この発明は薄層クロマトグラフィー質量分析装置に関す
るものである。
DETAILED DESCRIPTION OF THE INVENTION [Industrial Field of Application] This invention relates to a thin layer chromatography mass spectrometer.

[従来の技術] 従来、薄層クロマトグラフィーにおいては、展開槽内で
試料を展開分離した後、薄層を水素炎検出器などを用い
た自動検出装置に移し、保持時間とピーク高を求めてい
た。
[Conventional technology] Conventionally, in thin layer chromatography, after a sample is developed and separated in a developing tank, the thin layer is transferred to an automatic detection device using a hydrogen flame detector, etc., and the retention time and peak height are determined. Ta.

[発明が解決しようとする問題点] しかしながら、従来の装置によると、展開槽と検出装置
とが別々であるため、操作が煩雑であり、また定性分析
を行なう手段はなかった。
[Problems to be Solved by the Invention] However, in the conventional apparatus, since the development tank and the detection device are separate, the operation is complicated, and there is no means for performing qualitative analysis.

本発明の目的は上記の問題点を解決し、薄層クロマトグ
ラフィーで展開された各スポットを直接高感度に検出す
ると共に、定性分析を行なうことのできる薄層クロマト
グラフィー質量分析装置を提供することにある。
An object of the present invention is to solve the above problems and provide a thin layer chromatography mass spectrometer that can directly detect each spot developed by thin layer chromatography with high sensitivity and perform qualitative analysis. It is in.

[問題点を解決するための手段] 本発明は展開溶媒を排出する展開溶媒排出配管、真空排
気配管およびガス供給配管がそれぞれ配設され、薄層上
の試料を展開分離する展開槽と、前記薄層を保持する薄
層ホルダーおよびこの薄層ホルダーを駆動させる駆動機
構が配設されたアームと、前記薄層に隣接して前記展開
槽内に配設され薄層上の試料をイオン化するRF放電装
置と、このRF放電装置に接続したイオン加速装置と、
このイオン加速装置に接続した質量分析装置と、この質
量分析装置に接続したイオン検出装置とを具備してなる
ことを特徴とする薄層クロマトグラフィー質量分析装置
である。
[Means for Solving the Problems] The present invention provides a developing tank which is provided with a developing solvent discharge pipe for discharging a developing solvent, a vacuum exhaust pipe, and a gas supply pipe, and which develops and separates a sample on a thin layer; a thin layer holder for holding the thin layer; an arm provided with a drive mechanism for driving the thin layer holder; and an RF radio waves disposed in the development tank adjacent to the thin layer for ionizing the sample on the thin layer. a discharge device; an ion accelerator connected to the RF discharge device;
This thin layer chromatography mass spectrometer is characterized by comprising a mass spectrometer connected to the ion accelerator and an ion detection device connected to the mass spectrometer.

[作 用] この発明の要旨とするところは、薄層クロマトグラフィ
ーにおいて展開を行なった薄層上の各試料を、直接展開
槽内部に配設されたRF放電装置で検出し、質量分離を
行なうことであり、このために分析操作が簡単となる。
[Function] The gist of this invention is to detect each sample on a thin layer developed in thin layer chromatography with an RF discharge device disposed directly inside the development tank, and perform mass separation. This simplifies the analytical operation.

また、検出器に質量分析装置を用いているために、各ス
ポットの定性分析を行なうことができる。
Furthermore, since a mass spectrometer is used as a detector, qualitative analysis of each spot can be performed.

[実施例] 次に本発明を実施例によって説明する。[Example] Next, the present invention will be explained by examples.

第1図は本発明の薄層クロマトグラフィー質量分析装置
の一実施例を示す概略図である。
FIG. 1 is a schematic diagram showing an embodiment of the thin layer chromatography mass spectrometer of the present invention.

展開溶媒8を収容する展開槽14底部には、バルブ13
が介挿された展開溶媒排出配管16が配設されており、
展開溶媒8を展開槽14から排出できるようになってい
る。展開槽14にはこの他、真空ポンプ15に接続し、
バルブ12が介挿された真空排気配管17およびアルゴ
ンガスを供給し、バルブ11が介挿されたガス供給配管
18が配設されている。試料を展開する薄層1は、展開
槽4内部に垂直に立設されているアーム9の下方に配設
された薄層ホルダー19により保持され、かつこのアー
ム9に接続したステップモータ10によって薄層ホルダ
ー19と共に上下方向に可動とされている。また、薄層
1に隣接してRFコイル3、ホローカソード2およびア
ノード4よりなるRF放電装置20が展開槽内部に配設
され、薄層表面をスパッタして試料をイオン化させる。
A valve 13 is installed at the bottom of the development tank 14 that accommodates the development solvent 8.
A developing solvent discharge pipe 16 is provided, in which a developing solvent discharge pipe 16 is inserted.
The developing solvent 8 can be discharged from the developing tank 14. In addition to this, the development tank 14 is connected to a vacuum pump 15,
A vacuum exhaust pipe 17 in which a valve 12 is inserted and a gas supply pipe 18 for supplying argon gas and in which a valve 11 is inserted are provided. The thin layer 1 on which the sample is developed is held by a thin layer holder 19 disposed below an arm 9 that stands vertically inside the developing tank 4, and the thin layer 1 is thinned by a step motor 10 connected to this arm 9. It is movable in the vertical direction together with the layer holder 19. Further, an RF discharge device 20 consisting of an RF coil 3, a hollow cathode 2, and an anode 4 is disposed adjacent to the thin layer 1 inside the developing tank, and sputters the surface of the thin layer to ionize the sample.

RF放電装置20にはイオン加速電極5が備えられたイ
オン加速装置21、Qポール質量分析装置6およびイオ
ン検出装置7が順に配設されている。
An ion accelerator 21 equipped with an ion accelerating electrode 5, a Q-pole mass spectrometer 6, and an ion detector 7 are arranged in the RF discharge device 20 in this order.

次に以上のように構成された薄層クロマトグラフィー質
量分析装置の動作について述べる。
Next, the operation of the thin layer chromatography mass spectrometer configured as described above will be described.

試料を薄層1上に載せ、この薄層1を薄層ホルダー19
に取り付ける。次いでこの薄層1を、ステップモータ1
0によって展開槽14内の展開溶媒8に薄層1の下部が
浸漬されるまで下ろし、試料の展開を行なう。展開が終
了したらバルブ13を開き、展開溶媒8を展開槽14外
に放出する。次にバルブ13を閉め、次いでバルブ12
を開き、真空ポンプ15により展開槽14内を真空排気
する。このときに、薄層1の乾燥も行なわれる。展開槽
14内が十分な真空になったらバルブ11を開き、展開
槽14内にArガスを1 X 1o−4rorr程度リ
ークする。次にホローカソード2およびアノード4に電
圧をかけ、RF電源よりRFコイル3に高周波電力をか
けることにより、ホローカソード2内にRFプラズマを
形成する。形成されたRFプラズマにより、薄層表面が
スパッタされ、展開された試料がイオン化する。イオン
は、アノード4中夫の穴から引き出されてイオン加速装
置21に導入され、イオン加速電極5により加速されて
Qポール質量分析装置6に入射する。質量分離されたイ
オンは、イオン検出装置7によって検出される。このよ
うにして1回のマス−スキャンが終了した時点で、薄層
1はステップモータ10により2mm程度上方に移動さ
れ、薄層1の次の部分が質量分析される。このようにし
て、薄層の各部分から分離された試料は質量分析装置に
より検出され、定性分析が行なわれる。
A sample is placed on the thin layer 1, and this thin layer 1 is placed on the thin layer holder 19.
Attach to. This thin layer 1 is then passed through a step motor 1
0 until the lower part of the thin layer 1 is immersed in the developing solvent 8 in the developing tank 14, and the sample is developed. When the development is completed, the valve 13 is opened and the development solvent 8 is discharged to the outside of the development tank 14. Next, close valve 13, then close valve 12.
is opened, and the inside of the development tank 14 is evacuated by the vacuum pump 15. At this time, the thin layer 1 is also dried. When the inside of the development tank 14 becomes sufficiently vacuum, the valve 11 is opened and Ar gas is leaked into the development tank 14 at a rate of about 1×1o-4 rorr. Next, an RF plasma is formed in the hollow cathode 2 by applying a voltage to the hollow cathode 2 and the anode 4 and applying high frequency power to the RF coil 3 from the RF power source. The formed RF plasma sputters the surface of the thin layer and ionizes the developed sample. Ions are extracted from the hole in the anode 4 and introduced into the ion accelerator 21, accelerated by the ion accelerating electrode 5, and incident on the Q-pole mass spectrometer 6. The mass-separated ions are detected by an ion detection device 7. When one mass scan is completed in this manner, the thin layer 1 is moved upward by about 2 mm by the step motor 10, and the next portion of the thin layer 1 is subjected to mass analysis. In this way, the samples separated from each part of the thin layer are detected by a mass spectrometer and subjected to qualitative analysis.

次にこの装置を用いて有機化合物を分析した結果、高感
度で各ピークが検出され同時に定性分析を行なうことも
できた。
Next, when organic compounds were analyzed using this device, each peak was detected with high sensitivity, and qualitative analysis could also be performed at the same time.

[発明の効果] 以上説明したように、本発明の薄層クロマトグラフィー
質量分析装置によれば薄層展開された各試料を直接展開
槽内の検出装置に導入して質量分析による定性分析を行
なうので分析操作が簡略化されると共に、各試料を高感
度で検出することができる。
[Effects of the Invention] As explained above, according to the thin layer chromatography mass spectrometer of the present invention, each sample developed in a thin layer is directly introduced into the detection device in the development tank to perform qualitative analysis by mass spectrometry. Therefore, the analysis operation is simplified and each sample can be detected with high sensitivity.

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

第1図は本発明の一実施例を示す概略図である。 1・・・薄層       2・・・ホローカソード3
・・・RFコイル    4・・・アノード5・・・イ
オン加速電極 6・・・Qポール質量分析装置 7・・・イオン検出装置  8・・・展開溶媒9・・・
アーム      10・・・ステップモータ11、1
2.13・・・バルブ  14・・・展開槽15・・・
真空ポンプ    16・・・展開溶媒排出配管17・
・・真空排気配管   18・・・ガス供給配管19・
・・薄層ホルダー   20・・・RF放電装置21・
・・イオン加速装置
FIG. 1 is a schematic diagram showing an embodiment of the present invention. 1... Thin layer 2... Hollow cathode 3
...RF coil 4...Anode 5...Ion accelerating electrode 6...Q pole mass spectrometer 7...Ion detection device 8...Developing solvent 9...
Arm 10...Step motor 11, 1
2.13...Valve 14...Development tank 15...
Vacuum pump 16...Developing solvent discharge piping 17.
・・Vacuum exhaust piping 18・・Gas supply piping 19・
...Thin layer holder 20...RF discharge device 21.
・Ion accelerator

Claims (1)

【特許請求の範囲】[Claims] (1)展開溶媒を排出する展開溶媒排出配管、真空排気
配管およびガス供給配管がそれぞれ配設され、薄層上の
試料を展開分離する展開槽と、前記薄層を保持する薄層
ホルダーおよびこの薄層ホルダーを駆動させる駆動機構
が配設されたアームと、前記薄層に隣接して前記展開槽
内に配設され薄層上の試料をイオン化するRF放電装置
と、このRF放電装置に接続したイオン加速装置と、こ
のイオン加速装置に接続した質量分析装置と、この質量
分析装置に接続したイオン検出装置とを具備してなるこ
とを特徴とする薄層クロマトグラフィー質量分析装置。
(1) A developing solvent discharge pipe for discharging the developing solvent, a vacuum exhaust pipe, and a gas supply pipe are respectively arranged, a developing tank for developing and separating the sample on the thin layer, a thin layer holder for holding the thin layer, and an arm provided with a drive mechanism for driving the thin layer holder; an RF discharge device disposed in the development tank adjacent to the thin layer for ionizing the sample on the thin layer; and connected to the RF discharge device. 1. A thin layer chromatography mass spectrometer comprising: an ion accelerator, a mass spectrometer connected to the ion accelerator, and an ion detection device connected to the mass spectrometer.
JP61052865A 1986-03-10 1986-03-10 Thin layered chromatography mass analyser Pending JPS62209352A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP61052865A JPS62209352A (en) 1986-03-10 1986-03-10 Thin layered chromatography mass analyser

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP61052865A JPS62209352A (en) 1986-03-10 1986-03-10 Thin layered chromatography mass analyser

Publications (1)

Publication Number Publication Date
JPS62209352A true JPS62209352A (en) 1987-09-14

Family

ID=12926761

Family Applications (1)

Application Number Title Priority Date Filing Date
JP61052865A Pending JPS62209352A (en) 1986-03-10 1986-03-10 Thin layered chromatography mass analyser

Country Status (1)

Country Link
JP (1) JPS62209352A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109298123A (en) * 2018-04-23 2019-02-01 河北丰研翔科技发展限公司 A kind of novel thin layer chromatogram scanner and the analysis method using the scanner

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109298123A (en) * 2018-04-23 2019-02-01 河北丰研翔科技发展限公司 A kind of novel thin layer chromatogram scanner and the analysis method using the scanner

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