JPH02181648A - Fluorescence detector for liquid chromatography - Google Patents
Fluorescence detector for liquid chromatographyInfo
- Publication number
- JPH02181648A JPH02181648A JP34889A JP34889A JPH02181648A JP H02181648 A JPH02181648 A JP H02181648A JP 34889 A JP34889 A JP 34889A JP 34889 A JP34889 A JP 34889A JP H02181648 A JPH02181648 A JP H02181648A
- Authority
- JP
- Japan
- Prior art keywords
- wavelength
- fluorescence
- excitation
- liquid chromatography
- fluorescence detector
- 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
Links
Landscapes
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
(57)【要約】本公報は電子出願前の出願データであるた
め要約のデータは記録されません。(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、蛍光法による液体クロマトグラフ用の検知器
に係り、特に、高感度測定に最適な、液体クロマトグラ
フ用蛍光検知器に関する。DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention relates to a detector for liquid chromatographs using a fluorescence method, and particularly to a fluorescence detector for liquid chromatographs that is most suitable for high-sensitivity measurements.
従来の装置は、日立テクニカルデータＦＬシートＮα２
７に記載されているように、あらかじめ、波長切替時間
、励起、蛍光波長をプログラムし、測定開始後、設定さ
れている切替時間どおりに、波長を切替えるようになっ
ている。The conventional device is Hitachi Technical Data FL Sheet Nα2
7, the wavelength switching time, excitation, and fluorescence wavelengths are programmed in advance, and after the start of measurement, the wavelengths are switched according to the set switching times.
上記従来技術は、測定ごとくクロマトピークの保持時間
が、溶媒のわずかな変化などによりずれた場合、波長切
替えが、ピークの途中で行われる可能性について十分考
慮されていない。本発明の目的は、測定ごとにクロマト
ピークの保持時間にずれがあった場合でも、常に波長切
替えは、クロマトグラフが谷の部分にある間に行われる
ようにすることにある。The above-mentioned conventional technology does not sufficiently consider the possibility that wavelength switching may be performed in the middle of a peak when the retention time of a chromatographic peak is shifted due to a slight change in the solvent or the like during measurement. An object of the present invention is to always perform wavelength switching while the chromatograph is in the trough even if there is a difference in the retention time of the chromatographic peak from measurement to measurement.
上記目的は、あらかじめ設定されていた波長切替え時間
が経過後、クロマトグラムをモニタしながら、谷の部分
で、自動的に波長を切替えるようにすることにより、達
成される。The above object is achieved by automatically switching the wavelength at the valley portion while monitoring the chromatogram after a preset wavelength switching time has elapsed.
あらかじめ設定された時間のみを使って波長を切替えた
場合には、特に近接したピークについて測定ごとの保持
時間のずれにより、ピーク途中に波長切替えが実行され
る場合があるが、これに、谷の部分を自動検知して、設
定時間経過後の条件と組合わせることにより、近接した
ピーク間でも常に谷の部分で、波長切替えを行うことが
できるようになる。If the wavelength is switched using only a preset time, wavelength switching may occur in the middle of the peak due to differences in retention time between measurements, especially for closely spaced peaks. By automatically detecting the area and combining it with the condition after the set time has elapsed, wavelength switching can always be performed at the valley part even between adjacent peaks.
以下、本発明の一実施例を図により説明する。 Hereinafter, one embodiment of the present invention will be described with reference to the drawings.
第１図において、光源１から出た光は励起側分光器２で
波長を選択された後、フローセル３に照射される。フロ
ーセル３には液体クロマトグラフのポンプにより、サン
プルが環流されている。フローセルから出た蛍光は、蛍
光側分光器４によって波長を選択された後、検知系５で
強度を測定される。ここで、励起側分光器２．蛍光側分
光器４は波長制御系６により制御されており、あらかじ
め波長切替え時間、励起、蛍光波長の設定値が、波長制
御系６に記憶されている。また、検知系５の出力も、波
長制御系６によってモニタされており、測定中の波長切
替えは、次のようにして行われる。In FIG. 1, the wavelength of light emitted from a light source 1 is selected by an excitation side spectrometer 2, and then irradiated onto a flow cell 3. A sample is refluxed into the flow cell 3 by a liquid chromatograph pump. The wavelength of the fluorescence emitted from the flow cell is selected by a fluorescence spectrometer 4, and then the intensity is measured by a detection system 5. Here, the excitation side spectrometer 2. The fluorescence side spectrometer 4 is controlled by a wavelength control system 6, and set values for wavelength switching time, excitation, and fluorescence wavelength are stored in advance in the wavelength control system 6. The output of the detection system 5 is also monitored by the wavelength control system 6, and wavelength switching during measurement is performed as follows.
測定開始後、設定されている波長切替え時間経過後に、
検知系５のモニタにより、現在クロマトグラムの谷にあ
り、波長切替可能かどうか確認される。不可能ならば、
可能となるまで待ち、可能となった時間に、波長切替え
を行う。After starting the measurement and after the set wavelength switching time has elapsed,
By monitoring the detection system 5, it is confirmed whether the chromatogram is currently in the trough and wavelength switching is possible. If it is not possible,
Wait until it becomes possible, and then switch the wavelength.
谷の検知は、一定のサンプリング間隔（１）を設定し、
ｔに対するデータ値の変化（ΔＩ）が、一定値以下にな
ったことを確認することにより行う。本実施例によれば
、各ピークに対する保持時間が、測定ごとにずれた場合
でも、谷検知の併用により、ピーク途中で波長切替えが
行われ、１回分のデータが使用できなくなるということ
は起こらない、また、保持時間を常に一定に保つように
、各条件を厳密に管理する必要もなくなる。To detect the valley, set a constant sampling interval (1),
This is done by confirming that the change in data value (ΔI) with respect to t is below a certain value. According to this example, even if the retention time for each peak deviates from measurement to measurement, by using valley detection in combination, the wavelength will be switched in the middle of the peak, and the data for one time will not become unusable. Moreover, it is no longer necessary to strictly control each condition so as to keep the holding time constant.
本発明によれば、測定ごとのクロマトグラム保持時間の
ずれに関係なく、常に安定した測定が行えるようになり
、測定の失敗を失くすことができる効果がある。According to the present invention, stable measurements can be performed at all times regardless of differences in chromatogram retention time between measurements, and measurement failures can be eliminated.
第１図は本発明の一実施例を示す図、第２図は蛍光強度
と時間の関係を示す図である。
１・・・光源、２・・・励起側分光器、３・・・フロー
セル、４・・・蛍光側分光器、５・・・検知系、６・・
・波長制御系。
第１図
１２図FIG. 1 is a diagram showing an embodiment of the present invention, and FIG. 2 is a diagram showing the relationship between fluorescence intensity and time. DESCRIPTION OF SYMBOLS 1... Light source, 2... Excitation side spectrometer, 3... Flow cell, 4... Fluorescence side spectrometer, 5... Detection system, 6...
・Wavelength control system. Figure 1 Figure 12
Claims (1)
プルを環流させるフローセルと、サンプルからの蛍光を
選択する蛍光側分光器と、蛍光強度を測定する検出系と
、あらかじめ、波長切替え時間、励起波長、蛍光波長を
記憶させ、測定中に自動的に切替えを制御する波長制御
系を有する蛍光検知器において、あらかじめ設定されて
いた波長切替え時間が経過後、クロマトグラムのピーク
をモニタし、クロマトグラムの谷になつたことを自動的
に検知し、波長を相替えることを特徴とする液体クロマ
トグラフ用蛍光検知器。1. A light source, an excitation side spectrometer that selects the excitation wavelength, a flow cell that circulates the sample, a fluorescence side spectrometer that selects the fluorescence from the sample, a detection system that measures the fluorescence intensity, and a wavelength switching time in advance. , in a fluorescence detector that has a wavelength control system that stores excitation wavelength and fluorescence wavelength and automatically controls switching during measurement, monitors the peak of the chromatogram after a preset wavelength switching time has elapsed, A fluorescence detector for liquid chromatography that automatically detects when a chromatogram reaches a valley and changes the wavelength.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP34889A JPH02181648A (en) | 1989-01-06 | 1989-01-06 | Fluorescence detector for liquid chromatography |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP34889A JPH02181648A (en) | 1989-01-06 | 1989-01-06 | Fluorescence detector for liquid chromatography |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH02181648A true JPH02181648A (en) | 1990-07-16 |
Family
ID=11471345
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP34889A Pending JPH02181648A (en) | 1989-01-06 | 1989-01-06 | Fluorescence detector for liquid chromatography |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH02181648A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011092766A1 (en) * | 2010-01-28 | 2011-08-04 | 株式会社 日立ハイテクノロジーズ | Spectrophotofluorometer and fluorescence detector for liquid chromatograph |
| WO2017149794A1 (en) * | 2016-03-01 | 2017-09-08 | 株式会社島津製作所 | Chromatograph device |
| CN107525878A (en) * | 2016-06-21 | 2017-12-29 | 中国科学院大连化学物理研究所 | A Fluorescent Detection Cell Holder for High Performance Liquid Chromatography and Flow Injection Analysis |
-
1989
- 1989-01-06 JP JP34889A patent/JPH02181648A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011092766A1 (en) * | 2010-01-28 | 2011-08-04 | 株式会社 日立ハイテクノロジーズ | Spectrophotofluorometer and fluorescence detector for liquid chromatograph |
| JP2011153945A (en) * | 2010-01-28 | 2011-08-11 | Hitachi High-Technologies Corp | Spectrofluorometer and fluorescence detector for liquid chromatograph |
| WO2017149794A1 (en) * | 2016-03-01 | 2017-09-08 | 株式会社島津製作所 | Chromatograph device |
| JPWO2017149794A1 (en) * | 2016-03-01 | 2018-10-18 | 株式会社島津製作所 | Chromatographic equipment |
| CN107525878A (en) * | 2016-06-21 | 2017-12-29 | 中国科学院大连化学物理研究所 | A Fluorescent Detection Cell Holder for High Performance Liquid Chromatography and Flow Injection Analysis |
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