JPH0339730Y2 - - Google Patents
Info
- Publication number
- JPH0339730Y2 JPH0339730Y2 JP18792384U JP18792384U JPH0339730Y2 JP H0339730 Y2 JPH0339730 Y2 JP H0339730Y2 JP 18792384 U JP18792384 U JP 18792384U JP 18792384 U JP18792384 U JP 18792384U JP H0339730 Y2 JPH0339730 Y2 JP H0339730Y2
- Authority
- JP
- Japan
- Prior art keywords
- column
- guard column
- mobile phase
- liquid chromatograph
- packing material
- 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
Links
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 13
- 239000000463 material Substances 0.000 claims description 9
- 238000012856 packing Methods 0.000 claims description 8
- 239000000377 silicon dioxide Substances 0.000 claims description 7
- 150000002009 diols Chemical class 0.000 claims description 6
- 238000004458 analytical method Methods 0.000 description 8
- 239000000356 contaminant Substances 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- 239000012062 aqueous buffer Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000010494 dissociation reaction Methods 0.000 description 3
- 230000005593 dissociations Effects 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 3
- 239000000243 solution Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- LWIHDJKSTIGBAC-UHFFFAOYSA-K tripotassium phosphate Chemical compound [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 description 2
- 239000007983 Tris buffer Substances 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000004255 ion exchange chromatography Methods 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 238000004811 liquid chromatography Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 229920001184 polypeptide Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 229910000160 potassium phosphate Inorganic materials 0.000 description 1
- 235000011009 potassium phosphates Nutrition 0.000 description 1
- 102000004196 processed proteins & peptides Human genes 0.000 description 1
- 108090000765 processed proteins & peptides Proteins 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- SCPYDCQAZCOKTP-UHFFFAOYSA-N silanol Chemical compound [SiH3]O SCPYDCQAZCOKTP-UHFFFAOYSA-N 0.000 description 1
- 125000005372 silanol group Chemical group 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- LENZDBCJOHFCAS-UHFFFAOYSA-N tris Chemical compound OCC(N)(CO)CO LENZDBCJOHFCAS-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Treatment Of Liquids With Adsorbents In General (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Description
【考案の詳細な説明】
(イ) 産業上の利用分野
本考案は、液体クロマトグラフ分析において、
分析カラムを保護するためのガードカラムを備え
たクロマトグラフに関する。[Detailed explanation of the invention] (a) Industrial application field This invention is applicable to liquid chromatography analysis.
This invention relates to a chromatograph equipped with a guard column for protecting an analytical column.
(ロ) 従来技術
従来の液体クロマトグラフにおいては、ガード
カラムというのは試料導入部と分析カラムの間に
配置され、主として不可逆吸着を生ずる物質（分
析条件下での移動相では溶出しない成分）を吸着
させることを目的としていた。(b) Prior art In conventional liquid chromatographs, a guard column is placed between the sample introduction section and the analysis column, and is used to mainly prevent substances that cause irreversible adsorption (components that do not elute with the mobile phase under analysis conditions). It was intended to be absorbed.
また、ガードカラムの充てん剤としては分析カ
ラム充てん剤と同じタイプのものを使用してい
た。 In addition, the same type of packing material for the analytical column was used as the packing material for the guard column.
(ハ) 考案が解決しようとする問題点
最近の液体クロマトグラフでは、カラム充てん
剤の微粒化に伴い、装置の耐圧が要求されるため
各部分（カラム管材や流路）の素材として腐蝕し
にくいステンレスが用いられている。しかし、こ
のステンレスは、移動相として各種塩類を含む水
系緩衝液を使用する場合には経時的に腐蝕してい
き、長時間使用するといわゆる「さび」を生じさ
せていた。生じた「さび」は、分析カラム上端の
充てん剤ベツドに蓄積されカラム圧の上昇、カラ
ムの分離能力の低下など分析カラム性能を低下さ
せる現象を引き起こすに至り問題となることがあ
つた。(c) Problems that the invention aims to solve In recent liquid chromatographs, as the column packing material becomes atomized, the equipment is required to withstand pressure, so the materials of each part (column tube material and flow path) are less likely to corrode. Stainless steel is used. However, this stainless steel corrodes over time when an aqueous buffer solution containing various salts is used as a mobile phase, and when used for a long period of time, so-called "rust" occurs. The resulting ``rust'' accumulates in the packing bed at the top of the analytical column, causing problems such as an increase in column pressure and a decrease in the separation capacity of the column, which deteriorates the performance of the analytical column.
この問題は、特に、移動相として水系緩衝液を
必ず用いねばならない生体成分の分析には重大で
ある。 This problem is particularly serious in the analysis of biological components, which necessarily requires the use of an aqueous buffer as a mobile phase.
なお、各種塩類を含む溶液を移動相に用いる場
合は、塩類中の不純物は特級試薬といえども無視
できない場合がある。 Note that when a solution containing various salts is used as a mobile phase, impurities in the salts may not be ignored even if they are special grade reagents.
更に、従来のガードカラムは、インジエクタと
カラムの間に取りつけて使用していたので、装置
からの汚染物、移動相中の汚染物がともにガード
カラムにたまり、ひんぱんに取りかえる必要があ
つた。もちろん、試料中の汚染物も多い場合はガ
ードカラムの交換もさらにひんぱんに行わねばな
らなかつた。 Furthermore, since the conventional guard column was used by being attached between the injector and the column, contaminants from the device and contaminants in the mobile phase accumulated in the guard column, requiring frequent replacement. Of course, if there were many contaminants in the sample, the guard column had to be replaced more frequently.
(ニ) 問題点を解決するための手段
本考案は、上記に鑑みなされたもので、液体ク
ロマトグラフの試料導入部の前段に、水系GPC
用充てん剤、例えばジオールシリカを充てんして
なるガードカラムを配置することにより問題点を
一挙解決するものである。(d) Means for solving the problem The present invention was developed in view of the above, and it is possible to install an aqueous GPC at the front stage of the sample introduction section of the liquid chromatograph.
The problem can be solved at once by arranging a guard column filled with a filler such as diol silica.
(ホ) 作用
本考案の液体クロマトグラフは、試料導入部の
前段に配置したガードカラムにより、水系移動相
中に含まれる各種塩類によつて生じる汚染を防
ぎ、終局的には、分析カラムを保護する。(E) Function The liquid chromatograph of the present invention prevents contamination caused by various salts contained in the aqueous mobile phase by using a guard column placed before the sample introduction section, and ultimately protects the analytical column. do.
(ヘ) 実施例
本考案の液体クロマトグラフの基本的な構成の
１つの例を第１図に示す。（図１はアイソクラテ
イツクシステムだがグラジエントシステムでも可
能）
１が移動相液溜、２が送液ポンプ、３がガード
カラム、４が試料導入部、５が分析カラム、６が
検出器、７が記録計である。(F) Example One example of the basic configuration of the liquid chromatograph of the present invention is shown in FIG. (Figure 1 shows an isocratic system, but a gradient system is also possible.) 1 is a mobile phase reservoir, 2 is a liquid pump, 3 is a guard column, 4 is a sample introduction section, 5 is an analytical column, 6 is a detector, and 7 is a It is a recorder.
移動相液溜には、例えばたんぱく質分析の場合
には、トリス緩衝液（PH＝6.5〜7.5）などが、ポ
リペプチド分析の場合には、リン酸カリウム（PH
2.5）が用いられる。これら水系移動相を長時間
使用すると送液系から「さび」及び、移動相中の
不純物がカラム上部へ蓄積されるが、本考案では
ガードカラム３が配置されているため分析カラム
５へ影響を及ぼすことはない。 The mobile phase reservoir contains, for example, Tris buffer (PH = 6.5 to 7.5) for protein analysis, and potassium phosphate (PH = 6.5 to 7.5) for polypeptide analysis.
2.5) is used. When these aqueous mobile phases are used for a long time, "rust" from the liquid delivery system and impurities in the mobile phase accumulate in the upper part of the column, but in this invention, guard column 3 is installed so that there is no influence on analytical column 5. It will not affect you.
なお、本考案に使うガードカラム３の充てん剤
は、第２図ａに示す解離を起こさないように、水
系GPC用充てん剤、例えばジオールシリカを用
いる必要がある。ジオールシリカは、例えば、シ
リカゲルのｒ−グリシドキシプロピル化によつて
得られ、その表面は第２図ｂに示すようになつて
いる。第２図ｂより明らかなように、表面はシラ
ノールがキヤツプされ、アルコール性水酸基にな
つているため第２図ａのような解離は起こらな
い。 In addition, as the packing material for the guard column 3 used in the present invention, it is necessary to use an aqueous GPC packing material, such as diol silica, so as not to cause the dissociation shown in FIG. 2a. Diol silica is obtained, for example, by r-glycidoxypropylation of silica gel, and its surface is as shown in FIG. 2b. As is clear from FIG. 2b, silanol is capped on the surface and becomes alcoholic hydroxyl groups, so the dissociation as shown in FIG. 2a does not occur.
そのため、特にイオン交換クロマトグラフイー
などの場合のように、グラジエント分析の場合で
もガードカラムとしては最適である。 Therefore, it is especially suitable as a guard column even for gradient analysis, such as in ion exchange chromatography.
また、上記ジオールシリカは細孔径の大きいも
のの方が、残存シラトルが少ないため有効であ
る。 Furthermore, the diol silica having a larger pore diameter is more effective because it has less residual silatol.
(ト) 効果
本考案の液体クロマトグラフによれば、移動相
中の不総物及び長期にわたつて水系緩衝液を使用
することによる送液系からの汚染物（例えばさび
など）をガードカラムでトラツプできるので分析
カラムの長期にわたる安定な使用が可能である。(g) Effects According to the liquid chromatograph of the present invention, impurities in the mobile phase and contaminants (such as rust) from the liquid delivery system due to long-term use of an aqueous buffer can be removed using the guard column. Since it can be trapped, the analytical column can be used stably over a long period of time.
また、ガードカラムは、試料導入部の前に接続
されるため試料バンドの広がりに影響を及ぼすこ
とはない。 Furthermore, since the guard column is connected before the sample introduction section, it does not affect the spread of the sample band.
第１図は、本考案に係る液体クロマトグラフの
概略図、第２図(a)は、シリカ表面シラノール基の
解離図、第２図ｂは、ジオールシリカの表面図で
ある。
１…移動相液溜、３…ガードカラム、４…試料
導入部、５…分析カラム。
FIG. 1 is a schematic diagram of a liquid chromatograph according to the present invention, FIG. 2(a) is a dissociation diagram of silanol groups on the silica surface, and FIG. 2b is a surface diagram of diol silica. 1... Mobile phase reservoir, 3... Guard column, 4... Sample introduction part, 5... Analysis column.
Claims (1)
水系GPC用充てん剤を充てんしてなるガード
カラムを配置したことを特徴とする液体クロマ
トグラフ。 ２ 水系GPC充てん剤がジオールシリカである
実用新案登録請求の範囲第１項記載の液体クロ
マトグラフ。[Scope of claim for utility model registration] 1. In the front stage of the sample introduction part of the liquid chromatograph,
A liquid chromatograph characterized by having a guard column filled with an aqueous GPC packing material. 2. The liquid chromatograph according to claim 1, wherein the aqueous GPC packing material is diol silica.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP18792384U JPH0339730Y2 (en) | 1984-12-10 | 1984-12-10 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP18792384U JPH0339730Y2 (en) | 1984-12-10 | 1984-12-10 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS61102960U JPS61102960U (en) | 1986-07-01 |
| JPH0339730Y2 true JPH0339730Y2 (en) | 1991-08-21 |
Family
ID=30745398
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP18792384U Expired JPH0339730Y2 (en) | 1984-12-10 | 1984-12-10 |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0339730Y2 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2739527B2 (en) * | 1991-06-05 | 1998-04-15 | ジーエルサイエンス株式会社 | Device for removing impurities from eluent |
-
1984
- 1984-12-10 JP JP18792384U patent/JPH0339730Y2/ja not_active Expired
Also Published As
| Publication number | Publication date |
|---|---|
| JPS61102960U (en) | 1986-07-01 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Pedersen-Bjergaard et al. | Liquid− liquid− liquid microextraction for sample preparation of biological fluids prior to capillary electrophoresis | |
| Chladek et al. | Use of bonded phase silica sorbents for the sampling of priority pollutants in wastewaters | |
| Campíns-Falcó et al. | Column-switching techniques for high-performance liquid chromatography of drugs in biological samples | |
| Prosen et al. | Solid-phase microextraction | |
| Lee | Reversed-phase HPLC from pH 1 to 13 | |
| Ward et al. | Separation of enantiomers using vancomycin in a countercurrent process by suppression of electroosmosis | |
| Stroink et al. | On‐line sample preconcentration in capillary electrophoresis, focused on the determination of proteins and peptides | |
| US5863428A (en) | Guard cartridge for chromatography | |
| Lim et al. | Ammonium acetate: A general purpose buffer for clinical applications of high-performance liquid chromatography | |
| Di Corcia et al. | Extraction and isolation of phenoxy acid herbicides in environmental waters using two adsorbents in one minicartridge | |
| JPS62206444A (en) | Chromatography-pre-column | |
| Bombaugh et al. | High resolution preparative liquid chromatography using recycle | |
| JPH0339730Y2 (en) | ||
| US20030190757A1 (en) | Method and device for collecting and concentrating specimen | |
| Van Bruijnsvoort et al. | Determination of chlorophenols by micellar electrokinetic chromatography with electrochemical detection | |
| Eble et al. | Simplified description of high-performance liquid chromatographic separation under overload conditions, based on the Craig distribution model: II. Effect of isotherm type, and experimental verification of computer simulations for a single band | |
| Huber et al. | Enrichment of trace components from liquids by displacement column liquid chromatography | |
| US20060243651A1 (en) | Multi-velocity fluid channels in analytical instruments | |
| Eriksson et al. | Determination of catecholamines in urine by liquid chromatography and electrochemical detection after online sample purification on immobilized boronic acid | |
| Kirkland et al. | Rapid, high-resolution high-performance liquid chromatographic analysis of antibiotics | |
| Torres et al. | Purification of monoclonal antibodies by complex-displacement chromatography on CM-cellulose | |
| Miwa et al. | Application of an ovomucoid-conjugated polymer column for the enantiospecific determination of chlorprenaline concentrations in plasma | |
| Tagliaro et al. | Direct injection high-performance liquid chromatographic assay of morphine with electrochemical detection, a polymeric column and an alkaline eluent | |
| Whitehouse et al. | Separation of deoxyribonucleotides using ion suppression high performance liquid chromatography with a reversed-phase column | |
| Saner et al. | TRACE-ENRICHMENT TECHNIQUES FOR ORGANIC TRACE ANALYSIS |