JPH04301763A - High speed liquid chromatograph - Google Patents
High speed liquid chromatographInfo
- Publication number
- JPH04301763A JPH04301763A JP9129691A JP9129691A JPH04301763A JP H04301763 A JPH04301763 A JP H04301763A JP 9129691 A JP9129691 A JP 9129691A JP 9129691 A JP9129691 A JP 9129691A JP H04301763 A JPH04301763 A JP H04301763A
- Authority
- JP
- Japan
- Prior art keywords
- mobile phase
- precolumn
- impurities
- column
- analysis
- 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.)
- Withdrawn
Links
- 239000007788 liquid Substances 0.000 title claims abstract description 13
- 239000012535 impurity Substances 0.000 claims abstract description 18
- 238000002347 injection Methods 0.000 claims description 9
- 239000007924 injection Substances 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- 238000004458 analytical method Methods 0.000 abstract description 18
- 238000000034 method Methods 0.000 abstract description 8
- 238000010828 elution Methods 0.000 abstract description 6
- 238000006243 chemical reaction Methods 0.000 abstract 1
- 230000000717 retained effect Effects 0.000 description 5
- 239000002904 solvent Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000004128 high performance liquid chromatography Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000012459 cleaning agent Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000011002 quantification Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Landscapes
- Treatment Of Liquids With Adsorbents In General (AREA)
Abstract
Description
【０００１】0001
【産業上の利用分野】本発明は、高速液体クロマトグラ
フ、より詳しくはグラジェント法を適用時に生じるベー
スラインの補正技術に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to high performance liquid chromatography, and more particularly to a technique for correcting a baseline generated when applying a gradient method.
【０００２】0002
【従来の技術】高速液体クロマトグラフのベースライン
の補正は、移動相送液ポンプと試料注入機構の間にプレ
カラムを介装することにより行なわれているが、ベース
ラインを完全に補正するためにはプレカラムが分析用カ
ラムと同一の相互作用を有するとともに、分析用カラム
よりも挾雑物に対する強い保持力を備えてることが必要
であるが、このような条件は実際の装置に備えさせるこ
とは極めて困難である。[Prior Art] Baseline correction in high-performance liquid chromatographs is performed by interposing a precolumn between a mobile phase liquid pump and a sample injection mechanism, but in order to completely correct the baseline, It is necessary for the precolumn to have the same interaction as the analytical column and to have stronger retention power for contaminants than the analytical column, but these conditions cannot be provided in the actual equipment. It is extremely difficult.
【０００３】0003
【発明が解決しようとする課題】このため、現時点での
ベースライン補正用のプレカラムはベースラインの変動
を比較的小さく抑える程度の機能しか有せず、全てのピ
−クに対する妨害を除去することは極めて困難で、特に
時間とともに溶媒の組成が変化するグラジェント法を適
用した高速液体クロマトグラフにあっては、特定の組成
の移動相によりプレカラムに保持された挾雑物は、同時
に濃縮もされることにもなるから、移動相の溶出力が大
きくなった場合には、保持されていた挾雑物が溶出して
しまいベースラインを大きく変動させるという問題ある
。本発明はこのような問題に鑑みてなされたものであっ
て、その目的とするところはベースラインの変動を極め
て小さくすることができるグラジェント法を適用した高
速液体クロマトグラフを提供することである。[Problem to be Solved by the Invention] For this reason, the current precolumn for baseline correction only has the function of suppressing baseline fluctuations to a relatively small level, and it is difficult to eliminate interference with all peaks. This is extremely difficult, especially in high-performance liquid chromatography that uses a gradient method where the solvent composition changes over time. Therefore, when the elution power of the mobile phase increases, there is a problem in that retained impurities are eluted and the baseline fluctuates greatly. The present invention has been made in view of these problems, and its purpose is to provide a high-performance liquid chromatograph to which a gradient method is applied, which can extremely minimize fluctuations in the baseline. .
【０００４】0004
【課題を解決するための手段】このような問題を解消す
るために本発明においては、移動相の組成切換えに連動
する切換弁に、各移動相の不純物を保持するのに適した
複数のカラムを接続してなるプレカラム切換機構を、移
動相送液ポンプと試料注入機構の間に接続するようにし
た。[Means for Solving the Problems] In order to solve this problem, in the present invention, a plurality of columns suitable for retaining impurities in each mobile phase are installed in a switching valve that is linked to switching the composition of the mobile phase. A pre-column switching mechanism is connected between the mobile phase liquid transfer pump and the sample injection mechanism.
【０００５】[0005]
【作用】移動相の組成が変化する毎にその組成に適した
プレカラムが選択的に接続される一方、不純物を保持し
たプレカラムが分析流路から切り離されるため、直前の
組成の移動相で保持されている不純物が変更後の移動相
の溶出力により溶け出すのを確実に防止でき、これによ
りしてベースラインの変動が抑制されることになる。[Operation] Each time the composition of the mobile phase changes, a precolumn suitable for that composition is selectively connected, while the precolumn holding impurities is separated from the analysis flow path, so that the precolumn containing impurities is retained in the mobile phase with the previous composition. It is possible to reliably prevent impurities contained in the sample from leaching out due to the elution power of the changed mobile phase, thereby suppressing fluctuations in the baseline.
【０００６】[0006]
【実施例】次に本発明の詳細を図示した実施例に基づい
て説明する。図１は本発明の一実施例を示すものであっ
て、図中符号１は、ステップグラジェント用溶媒切換え
機構で、この実施例では３種類の移動相を収容するタン
ク１、２、３と、洗浄剤を収容したタンク４が接続され
て、制御装置６からの信号により弁を切換えて所定組成
の移動相タンク１、２、３、４をポンプ７に連通させる
ように構成されている。DESCRIPTION OF THE PREFERRED EMBODIMENTS Next, details of the present invention will be explained based on illustrated embodiments. FIG. 1 shows an embodiment of the present invention, and reference numeral 1 in the figure is a step gradient solvent switching mechanism, and in this embodiment, there are tanks 1, 2, and 3 containing three types of mobile phases. , a tank 4 containing a cleaning agent is connected, and the mobile phase tanks 1, 2, 3, and 4 having a predetermined composition are connected to the pump 7 by switching valves in response to a signal from a control device 6.
【０００７】１０は、プレカラム切換え機構で、図２に
示したように軸１１を中心に回動する第１の摺動面１２
と、軸の回転に関わりなく静止状態を維持する第２の摺
動面１３とを有する第１のバルブ１４と、同様の構造を
備える第２のバルブ１５とを、その静止側の摺動面を軸
１１で一定間隔に保持させるとともに、これらの摺動面
に各移動相の不純物を保持するのに適した複数のプレカ
ラム１６、１７を接続し、軸１１の回転により１つのプ
レカラムを選択的に分析流路に接続できるように構成さ
れている。Reference numeral 10 denotes a pre-column switching mechanism, which has a first sliding surface 12 that rotates around a shaft 11 as shown in FIG.
A first valve 14 having a second sliding surface 13 that maintains a stationary state regardless of rotation of the shaft, and a second valve 15 having a similar structure. are held at regular intervals by a shaft 11, and a plurality of pre-columns 16 and 17 suitable for retaining the impurities of each mobile phase are connected to these sliding surfaces, and one pre-column is selectively moved by rotating the shaft 11. It is configured so that it can be connected to the analysis flow path.
【０００８】再び図１に戻って、プレカラム切換え機構
１０は、その流入口が移動相送液ポンプ７に、排出口が
試料注入機構１８に連通させられ、この実施例では図中
符号実線、点線、及び一点鎖線で示す３つの流路を選択
できるように構成されている。なお、図中符号１９は、
試料注入機構に接続された分析用カラムを、また符号２
０は検出器をそれぞれ示す。Returning to FIG. 1 again, the precolumn switching mechanism 10 has an inlet communicating with the mobile phase liquid feeding pump 7 and an outlet communicating with the sample injection mechanism 18. In this embodiment, the solid line and the dotted line in the figure , and three channels shown by dashed lines can be selected. In addition, the reference numeral 19 in the figure is
The analytical column connected to the sample injection mechanism is also labeled 2.
0 indicates a detector, respectively.
【０００９】この実施例において移動相タンク２、３、
４に溶出力が順番に強くなる移動相を収容し、溶出力を
高めながら分析するモードを制御装置６に設定する。こ
のような準備が終了した段階でプレカラム切換え機構１
０を図中実線により示す状態に設定し、ポンプ７を作動
させる。これによりポンプ７により送出された移動相タ
ンク２からの移動相が第１のプレカラム１６を通過して
試料注入機構１８、分析用カラム１９に流入する。第１
の移動相に含まれている不純物は、第１のプレカラム１
６に保持されて下流側に移動するのを阻止される。この
状態で試料注入機構１８から試料を注入すると、移動相
とともに分析用カラム１９に流れ込み、第１の移動相に
より溶出される成分が順次、検出器２０に排出される。In this embodiment, mobile phase tanks 2, 3,
The control device 6 is set to a mode in which mobile phases having increasing elution power are stored in the cell 4 and the analysis is performed while increasing the elution power. Once these preparations are completed, the pre-column switching mechanism 1
0 to the state shown by the solid line in the figure, and the pump 7 is operated. As a result, the mobile phase from the mobile phase tank 2 sent out by the pump 7 passes through the first pre-column 16 and flows into the sample injection mechanism 18 and the analysis column 19. 1st
Impurities contained in the mobile phase of the first pre-column 1
6 and is prevented from moving downstream. When a sample is injected from the sample injection mechanism 18 in this state, it flows into the analytical column 19 together with the mobile phase, and components eluted by the first mobile phase are sequentially discharged to the detector 20.
【００１０】このようにして第１の移動相により溶出さ
せるべき成分のピ−クが全て検出された時点で、制御装
置６により溶媒切換え機構１により第２の移動相タンク
３が選択される。同時にプレカラム切換え機構１０も制
御装置６からの信号を受けて、図中点線により示す流路
が選択される。この結果、第１のプレカラム１６が分析
流路から切り離され、代って第２のプレカラム１７が分
析流路に接続されることになる。これにより、第１のプ
レカラム１６に保持されている不純物は、溶出度の強い
第２の移動相に晒されることがなく、分析流路に溶出し
ない。[0010] In this way, when all the peaks of the components to be eluted by the first mobile phase are detected, the second mobile phase tank 3 is selected by the solvent switching mechanism 1 by the control device 6. At the same time, the pre-column switching mechanism 10 also receives a signal from the control device 6, and selects the flow path indicated by the dotted line in the figure. As a result, the first precolumn 16 is separated from the analysis flow path, and the second precolumn 17 is connected to the analysis flow path instead. Thereby, the impurities held in the first pre-column 16 are not exposed to the second mobile phase having a strong elubility and are not eluted into the analysis channel.
【００１１】第２のプレカラム１７が接続されると、第
２の移動相タンク３の移動相は、第２のプレカラム１７
により不純物を保持されて分析用カラム１９に流入する
。これにより、検出器２０は第１のプレカラム１６に保
持された不純物の流入を受けることなく、第２の移動相
タンク３により分析用カラム１９から溶出される成分を
検出することになる。この結果、ベースラインの変動を
受けないピ−ク波形を得ることができる。When the second pre-column 17 is connected, the mobile phase in the second mobile phase tank 3 is transferred to the second pre-column 17.
impurities are retained and flowed into the analytical column 19. Thereby, the detector 20 detects the components eluted from the analytical column 19 by the second mobile phase tank 3 without receiving the impurities held in the first pre-column 16. As a result, a peak waveform that is not affected by baseline fluctuations can be obtained.
【００１２】さらに第３の移動相タンク４が選択される
と、プレカラム切換え機構１０が制御装置６からの信号
を受けて図中一点鎖線で示す第３の流路に切換えられる
。これにより第２のプレカラム１７は、分析流路から切
り離されることになる。この結果、最も溶出力が強い移
動相が分析用カラム１９に流れ込み、分析用カラム１９
に保持されている残存成分を溶出させることになる。
もとより、プレカラム１６、１７がともに分析流路から
切り離されているため、プレカラム１６、１７に保持さ
れている不純物が検出器２０に流れ込むようなことがな
く、したがってベースラインの安定したピ−ク波形を得
ることができる。Further, when the third mobile phase tank 4 is selected, the precolumn switching mechanism 10 receives a signal from the control device 6 and switches to the third flow path shown by the dashed line in the figure. This causes the second precolumn 17 to be separated from the analysis flow path. As a result, the mobile phase with the strongest elution power flows into the analytical column 19.
The remaining components retained in the sample will be eluted. Since the pre-columns 16 and 17 are both separated from the analysis flow path, impurities retained in the pre-columns 16 and 17 do not flow into the detector 20, and therefore the baseline has a stable peak waveform. can be obtained.
【００１３】分析工程が終了すると、制御装置６は、第
４の移動相タンク５を選択して分析流路に洗浄液を供給
して分析用カラム１９を洗浄し、以下所定時間の経過後
にプレカラム切換え機構１０を作動させて第１、第２の
プレカラム１６、１７を分析流路に接続し、これに保持
されている不純物を排出させ、最初の状態に戻って次の
分析に備える。When the analysis process is completed, the control device 6 selects the fourth mobile phase tank 5 and supplies a washing liquid to the analysis flow path to wash the analysis column 19, and after a predetermined period of time has elapsed, the control device 6 switches the pre-column. The mechanism 10 is activated to connect the first and second precolumns 16 and 17 to the analysis flow path, discharge impurities held therein, and return to the initial state in preparation for the next analysis.
【００１４】なお、この実施例においてはステップグラ
ジェント法に例を採って説明したが、成分比が連続的に
変化する線形グラジェント法の場合においても、移動相
の溶出力が所定の強さに変化した段階でプレカラムを切
換えることにより同様の作用を奏することは明かである
。[0014] Although this example has been explained by taking the step gradient method as an example, even in the case of a linear gradient method in which the component ratio changes continuously, it is possible to It is clear that the same effect can be achieved by switching the precolumn at the stage when the condition changes.
【００１５】[0015]
【発明の効果】以上説明したように本発明においては、
移動相の組成切換えに連動する切換弁に、各移動相の不
純物を保持するのに適した複数のカラムを接続してなる
プレカラム切換機構を移動相送液ポンプと試料注入機構
の間に接続したので、移動相中に含まれる不純物を保持
したプレカラムを、移動相の組成が変更される度に分析
流路から切り離すことができ、特に移動相の溶出力が変
化するグラジェント法において生じ易いベースラインの
変動を確実に抑制して精度の高い定量を行なうことがで
きる。[Effects of the Invention] As explained above, in the present invention,
A pre-column switching mechanism, which consists of multiple columns suitable for retaining impurities in each mobile phase, is connected between the mobile phase liquid pump and the sample injection mechanism to a switching valve that changes the composition of the mobile phase. Therefore, the pre-column that retains impurities contained in the mobile phase can be separated from the analysis flow path every time the composition of the mobile phase is changed. It is possible to reliably suppress line fluctuations and perform highly accurate quantification.
【図１】本発明の一実施例を示す装置の構成図である。FIG. 1 is a configuration diagram of an apparatus showing an embodiment of the present invention.
【図２】同上装置にプレカラム切換え機構の一実施例を
示す図である。FIG. 2 is a diagram showing an embodiment of a pre-column switching mechanism in the same device.
１ ステップグラジェント用溶媒切換え機構２、３、
４、５ 移動相タンク
７ 移動相送液ポンプ
１０ プレカラム切換え機構
１６、１７ プレカラム
１８ 試料注入機構
１９ 分析用カラム1 Solvent switching mechanism for step gradient 2, 3,
4, 5 Mobile phase tank 7 Mobile phase liquid pump 10 Pre-column switching mechanism 16, 17 Pre-column 18 Sample injection mechanism 19 Analysis column
Claims (1)
に、移動相の不純物を保持するのに適した複数のカラム
を接続してなるプレカラム切換機構を移動相送液ポンプ
と試料注入機構の間に接続してなる高速液体クロマトグ
ラフ。Claim 1: A pre-column switching mechanism consisting of a plurality of columns suitable for retaining impurities in the mobile phase is connected to a switching valve linked to switching the composition of the mobile phase between the mobile phase liquid pump and the sample injection mechanism. A high-performance liquid chromatograph connected between
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP9129691A JPH04301763A (en) | 1991-03-29 | 1991-03-29 | High speed liquid chromatograph |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP9129691A JPH04301763A (en) | 1991-03-29 | 1991-03-29 | High speed liquid chromatograph |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH04301763A true JPH04301763A (en) | 1992-10-26 |
Family
ID=14022509
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP9129691A Withdrawn JPH04301763A (en) | 1991-03-29 | 1991-03-29 | High speed liquid chromatograph |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH04301763A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6601439B2 (en) * | 2001-07-05 | 2003-08-05 | Agilent Technologies, Inc. | Method of reducing baseline instabilities in liquid chromatographic measurements and liquid chromatography apparatus |
-
1991
- 1991-03-29 JP JP9129691A patent/JPH04301763A/en not_active Withdrawn
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6601439B2 (en) * | 2001-07-05 | 2003-08-05 | Agilent Technologies, Inc. | Method of reducing baseline instabilities in liquid chromatographic measurements and liquid chromatography apparatus |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| A300 | Application deemed to be withdrawn because no request for examination was validly filed |
Free format text: JAPANESE INTERMEDIATE CODE: A300 Effective date: 19980514 |