JPH0216447A - Thin-layer chromatography sheet and its production - Google Patents
Thin-layer chromatography sheet and its productionInfo
- Publication number
- JPH0216447A JPH0216447A JP16582888A JP16582888A JPH0216447A JP H0216447 A JPH0216447 A JP H0216447A JP 16582888 A JP16582888 A JP 16582888A JP 16582888 A JP16582888 A JP 16582888A JP H0216447 A JPH0216447 A JP H0216447A
- Authority
- JP
- Japan
- Prior art keywords
- sheet
- phase
- layer chromatography
- cao
- glass
- 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
- 238000004809 thin layer chromatography Methods 0.000 title claims abstract description 19
- 238000004519 manufacturing process Methods 0.000 title claims description 7
- 239000005373 porous glass Substances 0.000 claims abstract description 24
- 239000011521 glass Substances 0.000 claims description 20
- 239000000203 mixture Substances 0.000 claims description 17
- 239000011148 porous material Substances 0.000 claims description 16
- 238000005191 phase separation Methods 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 8
- 239000000853 adhesive Substances 0.000 abstract description 8
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 8
- 238000001514 detection method Methods 0.000 abstract description 8
- 238000011161 development Methods 0.000 abstract description 6
- 239000002253 acid Substances 0.000 abstract description 5
- 229910052681 coesite Inorganic materials 0.000 abstract description 4
- 229910052906 cristobalite Inorganic materials 0.000 abstract description 4
- 239000000377 silicon dioxide Substances 0.000 abstract description 4
- 235000012239 silicon dioxide Nutrition 0.000 abstract description 4
- 229910052682 stishovite Inorganic materials 0.000 abstract description 4
- 229910052905 tridymite Inorganic materials 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 3
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 abstract 2
- 238000000465 moulding Methods 0.000 abstract 2
- 230000009257 reactivity Effects 0.000 abstract 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract 1
- 229910052593 corundum Inorganic materials 0.000 abstract 1
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 12
- 238000010438 heat treatment Methods 0.000 description 8
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 6
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 230000001070 adhesive effect Effects 0.000 description 6
- 239000003463 adsorbent Substances 0.000 description 6
- 239000002904 solvent Substances 0.000 description 6
- 239000000758 substrate Substances 0.000 description 6
- 238000000926 separation method Methods 0.000 description 5
- 230000005526 G1 to G0 transition Effects 0.000 description 4
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 4
- 235000001014 amino acid Nutrition 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- -1 1038-30wt% Inorganic materials 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 150000001413 amino acids Chemical class 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 229920000768 polyamine Polymers 0.000 description 3
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- QNAYBMKLOCPYGJ-REOHCLBHSA-N L-alanine Chemical compound C[C@H](N)C(O)=O QNAYBMKLOCPYGJ-REOHCLBHSA-N 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000010306 acid treatment Methods 0.000 description 2
- 235000004279 alanine Nutrition 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000004587 chromatography analysis Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- KIDHWZJUCRJVML-UHFFFAOYSA-N putrescine Chemical compound NCCCCN KIDHWZJUCRJVML-UHFFFAOYSA-N 0.000 description 2
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 2
- ATHGHQPFGPMSJY-UHFFFAOYSA-N spermidine Chemical compound NCCCCNCCCN ATHGHQPFGPMSJY-UHFFFAOYSA-N 0.000 description 2
- PFNFFQXMRSDOHW-UHFFFAOYSA-N spermine Chemical compound NCCCNCCCCNCCCN PFNFFQXMRSDOHW-UHFFFAOYSA-N 0.000 description 2
- 101100348017 Drosophila melanogaster Nazo gene Proteins 0.000 description 1
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 1
- 239000004471 Glycine Substances 0.000 description 1
- FFEARJCKVFRZRR-BYPYZUCNSA-N L-methionine Chemical compound CSCC[C@H](N)C(O)=O FFEARJCKVFRZRR-BYPYZUCNSA-N 0.000 description 1
- COLNVLDHVKWLRT-QMMMGPOBSA-N L-phenylalanine Chemical compound OC(=O)[C@@H](N)CC1=CC=CC=C1 COLNVLDHVKWLRT-QMMMGPOBSA-N 0.000 description 1
- KZSNJWFQEVHDMF-BYPYZUCNSA-N L-valine Chemical compound CC(C)[C@H](N)C(O)=O KZSNJWFQEVHDMF-BYPYZUCNSA-N 0.000 description 1
- RMOIHHAKNOFHOE-UHFFFAOYSA-N N-acetylcadaverine Chemical compound CC(=O)NCCCCCN RMOIHHAKNOFHOE-UHFFFAOYSA-N 0.000 description 1
- ONIBWKKTOPOVIA-UHFFFAOYSA-N Proline Natural products OC(=O)C1CCCN1 ONIBWKKTOPOVIA-UHFFFAOYSA-N 0.000 description 1
- 239000005700 Putrescine Substances 0.000 description 1
- KZSNJWFQEVHDMF-UHFFFAOYSA-N Valine Natural products CC(C)C(N)C(O)=O KZSNJWFQEVHDMF-UHFFFAOYSA-N 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000001917 fluorescence detection Methods 0.000 description 1
- HNDVDQJCIGZPNO-UHFFFAOYSA-N histidine Natural products OC(=O)C(N)CC1=CN=CN1 HNDVDQJCIGZPNO-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229930182817 methionine Natural products 0.000 description 1
- FEMOMIGRRWSMCU-UHFFFAOYSA-N ninhydrin Chemical compound C1=CC=C2C(=O)C(O)(O)C(=O)C2=C1 FEMOMIGRRWSMCU-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- COLNVLDHVKWLRT-UHFFFAOYSA-N phenylalanine Natural products OC(=O)C(N)CC1=CC=CC=C1 COLNVLDHVKWLRT-UHFFFAOYSA-N 0.000 description 1
- XNGIFLGASWRNHJ-UHFFFAOYSA-L phthalate(2-) Chemical compound [O-]C(=O)C1=CC=CC=C1C([O-])=O XNGIFLGASWRNHJ-UHFFFAOYSA-L 0.000 description 1
- 229920006267 polyester film Polymers 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 229940063673 spermidine Drugs 0.000 description 1
- 229940063675 spermine Drugs 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004474 valine Substances 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Abstract
Description
【発明の詳細な説明】
［産業上の利用分野コ
本発明は薄層クロマトクラフィーシート並びにその製造
法に関するものである。DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a thin layer chromatography sheet and a method for producing the same.
［従来の技術］
平滑なガラス板又はポリエステルフィルム（以下基板と
総称）上に、吸着剤の薄い層を付着させて固定相とし、
種々の溶媒（移動相）て試料を展開させる薄層クロマト
クラフィー（ＴＬＣ）は試料成分の分離、固定、定量等
に広く用いられている。[Prior art] A thin layer of adsorbent is attached onto a smooth glass plate or polyester film (hereinafter collectively referred to as the substrate) to serve as a stationary phase.
Thin layer chromatography (TLC), in which a sample is developed using various solvents (mobile phases), is widely used for separation, fixation, quantitative determination, etc. of sample components.
［発明か解決しようとする課題］
ＴＬＣはベーパークロマトクラフィーに比し展開時間も
短く、検出精度か良好である長所を有するか、次のよう
な問題点かある。[Problems to be Solved by the Invention] TLC has the advantages of shorter development time and better detection accuracy than vapor chromatography, but it has the following problems.
（１）吸着剤を基板に薄層ななして付着させるために接
着剤か使用されるか、反応性の強い検出試薬又は展開溶
媒を用いると吸着剤又は接着剤か侵され、吸着剤か基板
から剥離、脱落してしまうことかある。このため接着剤
を使わない薄層も使用されるが非常に脱落し易い。(1) If an adhesive is used to attach the adsorbent to the substrate in a thin layer, or if a highly reactive detection reagent or developing solvent is used, the adsorbent or adhesive will be attacked and the adsorbent or substrate will be damaged. It may peel off or fall off. For this reason, thin layers without adhesives are also used, but they tend to fall off very easily.
このため使用しつる展開溶媒及び検出試薬の種類が制限
される。This limits the types of developing solvents and detection reagents that can be used.
（２）展開、分離された試料の成分を検出試薬を用いて
同定、定量する際、吸着剤及び接着剤か検出試薬と反応
し、誤差を生ずることがある。(2) When identifying and quantifying components of a developed and separated sample using a detection reagent, the adsorbent and adhesive may react with the detection reagent, resulting in errors.
（３）展開、分離された試料の成分の付着している部分
を切り取り、次の段階の反応の原料或はＮＭＲ等の分析
試料として使用しようとすると、吸着剤の薄層粒子が基
板から剥離して使用でなくなる。(3) When trying to cut out the part of the developed and separated sample to which the components are attached and use it as a raw material for the next step of reaction or as an analysis sample for NMR, etc., the thin layer of adsorbent particles peels off from the substrate. It becomes unusable.
［課題を解決するための手段］
上記目的を達成するために、本発明においては、多数の
小孔を有する多孔質ガラスシート（以下本シートという
）を薄層クロマトグラフィーシートとして使用し、又Ｓ
ｉＯ２４５〜７０ｗｔ％、Ｂ２Ｏ．８〜３０ ｗｔ％、
ＣａＯ３〜２５ｗｔ％、Ａｌ２Ｏ３５〜１５ｗｔ％、
Ｎａ２Ｏ３〜８ ｗｔ％、Ｋ２Ｏ１〜５ｗｔ％、 Ｎａ
２Ｏ＋ Ｋ２Ｏ４〜ｌ ３ ｗｔ％、ＭｇＯ０〜８ｗｔ
％、又はＳｉＯ２４５〜７０ｗｔ％、Ｂ２Ｏ３８〜３０
ｗｔ％、ＣａＯ３〜２５ｗｔ％、Ａｌ２Ｏ３５〜ｌ ５
ｗｔ％なる組成を有するガラス成形体を熱処理してＢ２
Ｏ３、ＣａＯを主体とする相を分相せしめ、この相を溶
解除去することににより薄層クロマトクラフィーシート
を製造する。[Means for Solving the Problem] In order to achieve the above object, in the present invention, a porous glass sheet having a large number of small holes (hereinafter referred to as the present sheet) is used as a thin layer chromatography sheet, and S
iO245-70wt%, B2O. 8-30 wt%,
CaO3~25wt%, Al2O35~15wt%,
Na2O3-8 wt%, K2O1-5 wt%, Na
2O+ K2O4~l3wt%, MgO0~8wt
%, or SiO245-70wt%, B2O38-30
wt%, CaO3~25wt%, Al2O35~l 5
A glass molded body having a composition of wt% is heat-treated to form B2.
A thin layer chromatography sheet is manufactured by phase-separating a phase mainly composed of O3 and CaO, and dissolving and removing this phase.
次に、本発明を更に具体的に説明する。Next, the present invention will be explained in more detail.
本発明においては多孔質ガラスとしては、分相性を有す
るガラスを使用して得られる多孔質ガラス、特に３１０
２４５〜７０ｗｔ％、Ｂ、１０３８〜３０ｗｔ％、Ｃａ
Ｏ３〜２５ｗｔ％、Ａ１２Ｏｉ ５〜ｌ ５ ｗｔ％、
Ｎａ ２Ｏ３〜８ ｗ ｔ％、Ｋ２Ｏ１〜５ ｗｔ％、
ＮａｚＯ＋Ｋ２Ｏ４〜１３ｗｔ％、ＭｇＯ０〜８ｗｔ
％なる組成（組成Ａ）、又はＳｉＯ２４５〜７０ｗｔ％
、Ｂ２Ｏ：ｌ ８〜３０ｗｔ％、ＣａＯ３〜２５ｗｔ％
、Ａｌ２Ｏ３５〜１５ｗｔ％なる組成（組成り）を有す
るガラス成形体を熱処理してＢ２Ｏ３，ＣａＯを主体と
する相を分相せしめ、この相を溶解除去することにによ
って得られる多孔質ガラス（以下夫々多孔質ガラスＡ、
Ｂと呼ぶ）を用いるのが適当である。In the present invention, the porous glass is a porous glass obtained using a glass having a phase splitting property, particularly 310
245-70wt%, B, 1038-30wt%, Ca
O3~25wt%, A12Oi 5~l5wt%,
Na2O3-8 wt%, K2O1-5 wt%,
NazO+K2O4~13wt%, MgO0~8wt
% composition (composition A), or SiO2 45 to 70 wt%
, B2O:l 8-30wt%, CaO3-25wt%
A porous glass (hereinafter referred to as "porous glass") obtained by heat-treating a glass molded body having a composition (composition) of , Al2O35 to 15 wt% to separate a phase mainly composed of B2O3 and CaO, and dissolving and removing this phase. porous glass A,
B) is appropriate.
なお、本シートはブロック状のガラス成形体を分相処理
した後スライスし、得られたシートを酸処理することに
よって好適に製造することができる。In addition, this sheet can be suitably manufactured by subjecting a block-shaped glass molded body to phase separation treatment, slicing it, and treating the obtained sheet with an acid.
分相性を有するガラスとしては、組成Ａ又は組成りのガ
ラス（以下本ガラスと総称する）を使用するのか特に望
ましく、耐圧性か大きく、機械的強度が大であり、又耐
薬品性が大きく、ｐｕｏ〜１４の範囲で使用可能であり
、且つ孔径が均一であり、分離精度の大きい薄層クロマ
トグラフィーシートをうろことかできる。As the glass having phase separation, it is particularly desirable to use composition A or glass of composition (hereinafter collectively referred to as the present glass), which has high pressure resistance, high mechanical strength, and high chemical resistance. It can be used in the range of puo to 14, has a uniform pore size, and can be used to scale thin layer chromatography sheets with high separation accuracy.
なお組成Ａのガラスは小孔の径が３，０００〜１００．
０００人の範囲の小孔の径が比較的大きい多孔質ガラス
を得るために適し、又組成りのガラスは小孔の径か数百
〜２Ｏ，０００人の小孔の径が比較的小さい多孔質ガラ
スを得るのに適している。Note that the glass of composition A has a small pore diameter of 3,000 to 100 mm.
Suitable for obtaining porous glasses with relatively large pore diameters in the range of 1,000 to 20,000 pores; Suitable for obtaining quality glass.
以下本ガラス並びに本ガラスを使用した本シートの製造
法について、更に詳細に説明する。The present glass and the method for manufacturing the present sheet using the present glass will be described in more detail below.
本ガラスの成分のうちＳｉＯ２は分相、除去工程によっ
て得られる多孔硝子の骨格を形成するための基幹成分で
あり、Ａｌ２Ｏｆｆは補助成分として得られた多孔硝子
の脆さを減少させる作用を有する。Among the components of this glass, SiO2 is the basic component for forming the skeleton of the porous glass obtained by the phase separation and removal process, and Al2Off has the effect of reducing the brittleness of the porous glass obtained as an auxiliary component.
Ｂ２Ｏ３は一方において多孔硝子の骨格を形成する補助
成分として機能するが、他方ＣａＯと協同して、熱処理
によって微少な分相を生成する作用を有する。そしてこ
のようにして生成したＣａＯ１Ｂ２Ｏ３を主成分とする
分相を溶解除去することによって多孔質ガラスか形成さ
れる。On the one hand, B2O3 functions as an auxiliary component that forms the framework of the porous glass, but on the other hand, in cooperation with CaO, it has the effect of producing minute phase separation through heat treatment. A porous glass is formed by dissolving and removing the thus generated phase separation mainly composed of CaO1B2O3.
Ｂ２Ｏ３は上述の説明からも首肯しうるように細孔の大
きさを決定する重要な因子であり、分相中に移行して除
去されるＢ２Ｏ３量、或は逆に多孔硝子中に残存するＢ
２Ｏ３量は、細孔の径の均一性と密接な関係を有するこ
とが判明した。As can be seen from the above explanation, B2O3 is an important factor that determines the size of the pores, and the amount of B2O3 transferred and removed during phase separation, or conversely, the amount of B2O3 remaining in the porous glass.
It has been found that the amount of 2O3 has a close relationship with the uniformity of the pore diameter.
上記組成を有する調合原料を溶融し、所望形成の成形体
とする。成形体の製造方法に特に限定はなく常法を使用
することができる。The blended raw material having the above composition is melted to form a molded body of a desired shape. There are no particular limitations on the method for producing the molded body, and conventional methods can be used.
なおハツチの溶融中にＢ２Ｏ．の一部が揮発逸散するの
で、この逸散量を考慮してバッチ中のＢ２Ｏ３量を定め
ることが必要である。In addition, during the melting of the hatch, B2O. Since some of the B2O3 in the batch is volatilized and dissipated, it is necessary to determine the amount of B2O3 in the batch in consideration of this amount of dissipation.
組成Ａ又はＢを有するガラス（以下本ガラスという）よ
りなる成形体を熱処理してＣａｂ、 Ｂ２Ｏ：１を主
体とする相（以下Ｃａｂ、 Ｂ２Ｏ．相という）を分
相せしめる。加熱処理温度か高い程、又熱処理時間が長
い程ＣａＯ１Ｂ２Ｏ３相は大きくなる傾向を有し、熱処
理条件を選択することによって細孔の径を所望の値とす
ることがてきる。A molded body made of glass having composition A or B (hereinafter referred to as the present glass) is heat-treated to separate a phase mainly composed of Cab, B2O:1 (hereinafter referred to as Cab, B2O. phase). The higher the heat treatment temperature or the longer the heat treatment time, the larger the CaO1B2O3 phase tends to be. By selecting the heat treatment conditions, the diameter of the pores can be set to a desired value.
本ガラスを使用するときは均一な大きさの細孔を形成さ
せることができ、又処理条件、並びに組成の選択により
この径を５０〜１００，０００人の範囲とすることかで
きるか、この径を１．０００〜１２，０００人好ましく
は３．０００〜ａ、ｏｏｏ人とすることにより特に好適
な結果の得られることか判明した。加熱処理を行った本
ガラスよりなる成形体をスライスしてシート状となし次
いてこのシートを１１０１１１□ＳＯ，、Ｎｉ１．等の
酸中に浸漬してＣａＯ１Ｂ２Ｏ３相を溶解除去すること
により本シートを得ることかできる。なお酸処理を行な
うに先立ち、ＩＩＦ溶液で短時間その表面をエッチンク
処理するのか望ましい。When using this glass, pores with a uniform size can be formed, and the diameter can be set in the range of 50 to 100,000 by selecting the processing conditions and composition. It has been found that especially suitable results can be obtained by setting the number of people to 1,000 to 12,000 people, preferably 3,000 to a, ooo people. The molded body made of the heat-treated glass is sliced into a sheet, and then this sheet is coated with 110111□SO, Ni1. This sheet can be obtained by immersing the sheet in an acid such as the above to dissolve and remove the CaO1B2O3 phase. Note that before performing the acid treatment, it is desirable to etch the surface for a short time with an IIF solution.
前述したように熱処理の条件によって、得られる多孔硝
子の細孔の径を制御することができるが、細孔の径は多
孔質ガラス中に残存するＢ２Ｏ３の量に応じて変化する
こと及びこのＢ２Ｏ３の量は熱処理、酸処理の条件によ
って左右されることが判明した。モしてＢ２Ｏ３か望ま
しくは０．５ ｗｔ％以上残存するようこれらの条件を
定めることにより多孔硝子を薄層クロマトグラフ用シー
トとして使用した場合、特に好適な結果の得られること
が判明した。As mentioned above, the diameter of the pores in the resulting porous glass can be controlled by the conditions of heat treatment, but the diameter of the pores changes depending on the amount of B2O3 remaining in the porous glass, and this B2O3 It has been found that the amount of is influenced by the conditions of heat treatment and acid treatment. It has been found that particularly favorable results can be obtained when porous glass is used as a sheet for thin layer chromatography by setting these conditions such that preferably 0.5 wt% or more of B2O3 remains.
望ましい処理条件は次の通りである。Desirable processing conditions are as follows.
加熱温度 ６００〜８５０°Ｃ
加熱時間 ２〜４８ｈｒ、望ましくは１２〜４８ｈｒ酸
の種類 ＨＧＩ 、 Ｈ２ＳＯ，、Ｎ１（０３酸の濃度
０，０１〜２．ＯＮ、望ましくは０．１〜１．ＯＮ
処理時間 ２〜２Ｏｈｒ、望ましくは４〜１６ｈｒ温
度 ５０〜９５°Ｃ１望ましくは８０〜９０６Ｃ上記
のようにして得られた本シートを、各種の試料の成分の
分離、固定、定量に使用する。Heating temperature: 600-850°C Heating time: 2-48 hr, preferably 12-48 hr Type of acid: HGI, H2SO,, N1 (Concentration of 03 acid: 0.01-2.ON, preferably 0.1-1.ON) Treatment Time: 2~2Ohr, preferably 4~16hr
Temperature: 50-95°C, preferably 80-906°C The sheet obtained as described above is used for separating, fixing, and quantifying components of various samples.
次に本シートの使用法を説明する。Next, we will explain how to use this sheet.
本シートの寸法、厚みに特に限定はないか、２〜１０ｃ
ｍ×２〜１Ｏｃｔｌ、厚み０．２〜２１１１１１程度の
ものが好適に使用できる。このようなシートは充分な機
械的強度を有し、基板を用いて補強する必要はない。Is there any particular limitation on the dimensions and thickness of this sheet?2~10cm
A material having a size of m×2 to 1 octl and a thickness of about 0.2 to 211111 can be suitably used. Such sheets have sufficient mechanical strength and do not need to be reinforced with a substrate.
本シートの下部に試料を付着させ、本シートの下端を移
動相である液体中に浸漬する。移動相は本シート中に形
成されている多数の小孔中を毛細管現象によって上昇し
、本シート上部迄移動する。A sample is attached to the bottom of the sheet, and the bottom end of the sheet is immersed in the liquid that is the mobile phase. The mobile phase rises through the many small pores formed in the sheet by capillary action and moves to the top of the sheet.
この間に試料中に含まれる各成分は、移動相と固定相（
本シート）への分配係数に応じて分配移動され、各成分
への展開、分離か行われる。During this time, each component contained in the sample is separated from the mobile phase and stationary phase (
This sheet) is distributed and moved according to the distribution coefficient, and is expanded and separated into each component.
移動相は試料の種類、本シートの孔の大きさ等に応して
選択されるか、例えば、水、ピリジン、塩酸、硫醜、水
酸化ナトリウム溶液、ベンゼン、酢酸、クロロホルム等
を使用することかできる。The mobile phase may be selected depending on the type of sample, the size of the pores in the sheet, etc.; for example, water, pyridine, hydrochloric acid, sulfuric acid, sodium hydroxide solution, benzene, acetic acid, chloroform, etc. may be used. I can do it.
本シートを使用した場合の展開所要時間は数分ないし数
時間程度で、又分離性能も良好であり、ＴＬＣと同等以
上の性能を有する。When this sheet is used, the time required for development is about several minutes to several hours, and the separation performance is also good, and the performance is equal to or better than that of TLC.
又木シートは、ＴＬＣのように接着剤を用いていないの
で、各成分の展開、分離後、反応性の強い検出試薬を用
い、高温で、固定、定量を行うことができ、又接着剤に
起因する誤差を生ずることもない。In addition, the wood sheet does not use adhesives like TLC, so after developing and separating each component, it can be fixed and quantified at high temperature using a highly reactive detection reagent. There are no errors caused by this.
更に分離された各成分の付着したシートの所定部分を切
断し、次の反応、或は分析の試料として使用することも
できる。Furthermore, a predetermined portion of the sheet to which each separated component is attached can be cut and used as a sample for the next reaction or analysis.
［作 用］
多孔質ガラスシートをクロマトクラフィーの固定相とし
て利用し、試料の展開を該シート中で行うことにより、
固定相を補強する基板の使用を省くことを可能ならしめ
、接着剤の使用に起因する従来技術の欠点を解消する。[Function] By using a porous glass sheet as a stationary phase for chromatography and developing the sample in the sheet,
It makes it possible to dispense with the use of a substrate reinforcing the stationary phase and eliminates the drawbacks of the prior art due to the use of adhesives.
［実施例１］
■−ジメチルアミノナフタレンー５−スルフォニル（以
下ＤＮＳと略称）メチオニン、ＤＮＳバリン、ＤＮＳプ
ロリン、ＤＮＳ−ｔ＝！Ｊン、ＤＮＳグリシン、ＤＮＳ
アラニンの２．５ｘ １０−’Ｍのメタノール溶液を夫
々 ０．２ル旦ずつ、 ６，７００人の小孔の有する厚
み０．５ ｍｍ、５ ｃｎ＋Ｘ ５ ｃｍの大きさを有
するポーラスガラスシートの下から５ｍｍの点（原点）
にスポットした。これを展開槽内に置き、クロロホルム
で展開した。ドライヤーで風乾後、暗所にて２５４ｎｍ
の波長の紫外線を照射し、蛍光で、ＤＮＳアミノ酸の位
置を検出した。第１図はこのようにして得られたクロマ
トグラムであり、各アミノ酸はそれぞれよく分離した。[Example 1] ■-Dimethylaminonaphthalene-5-sulfonyl (hereinafter abbreviated as DNS) methionine, DNS valine, DNS proline, DNS-t=! Jn, DNS glycine, DNS
A 2.5 x 10-'M methanol solution of alanine was added at a rate of 0.2 l each under a porous glass sheet having a thickness of 0.5 mm and a size of 5 cm + x 5 cm with 6,700 pores. A point 5mm from (origin)
Spotted on. This was placed in a developing tank and developed with chloroform. After air drying with a hair dryer, 254nm in the dark
The position of the DNS amino acid was detected by fluorescence. FIG. 1 is a chromatogram obtained in this manner, in which each amino acid was well separated.
なお、展開は、図に示す溶媒先端の位置に溶媒が達する
迄行った。所要時間は１０１ｎであった。Incidentally, the development was carried out until the solvent reached the position of the solvent front shown in the figure. The required time was 101n.
［実施例２コ
実施例１と同じ実験を展開溶媒としてベンゼンと酢酸の
混液（１９：１．Ｖ／Ｖ）を用いて行った。[Example 2] The same experiment as in Example 1 was conducted using a mixture of benzene and acetic acid (19:1.V/V) as the developing solvent.
第２図はこのようにして得られたクロマトグラムである
。FIG. 2 is the chromatogram thus obtained.
［実施例３］
エチレンジアミン、プトレシン、スペルミジン、スペル
ミン、Ｎ−アセチルカダベリンの夫々のポリアミンを含
む２ Ｘ ｌ Ｏ−’Ｍの０．２ＭＮａＨＣＯｚの溶液
５０ＪＬｆＬに、２Ｘ１０−’ＭのＤＮＳ−ＣＩのアセ
トン溶液５０＋ａＱを加えて、３７℃で、３０分間反応
させた。反応液０．２ｇｌずつを６．７００人及び３，
１００人の小孔を有する実施例１と同じ大きさのポーラ
スガラスシートにスポットした。クロロホルムとピリジ
ンの混液（１：１゜ｖｉｖ ）て展開した。ポリアミン
のＤＮＳ誘導体の蛍光検出は実施例１と同しようにして
行った。第３図、第４図は夫々 ６，７００人、 ３，
１００人の小孔を有するシートを用いて得られたクロマ
トグラムである。図に示すように、ポリアミンのモノ、
ジおよびトリ、ＤＮＳ誘導体およびＤＮＳアミド（ＤＮ
Ｓ−ＮＨ２）などが分離した。６，７００人と ３，１
００人の小孔を有するシートの分離の差はみられないか
、展開速度か６ 、７００人のシートの方か早くて便利
であった。展開所要時間は夫々１０ｍ１眠２゜ｍｉｎて
あった。[Example 3] Acetone solution of 2×10-′M DNS-CI in 50 JLfL of 2×10-′M solution of 0.2M NaHCOz containing each polyamine of ethylenediamine, putrescine, spermidine, spermine, and N-acetylcadaverine. 50+aQ was added and reacted at 37°C for 30 minutes. 6.700 people and 3 people each received 0.2 g of the reaction solution.
The spots were placed on a porous glass sheet of the same size as in Example 1 having 100 small holes. It was developed with a mixture of chloroform and pyridine (1:1°viv). Fluorescence detection of the DNS derivative of polyamine was performed in the same manner as in Example 1. Figures 3 and 4 show 6,700 people, 3,
This is a chromatogram obtained using a sheet with 100 small holes. As shown in the figure, polyamine mono,
di and tri, DNS derivatives and DNS amides (DN
S-NH2) etc. were separated. 6,700 people and 3.1
There was no difference in separation between the sheets with holes for 6 and 700 people, and the spread speed was faster and more convenient. The time required for deployment was 10 m/2° min.
［実施例４］
フェニルアラニンおよびアラニンを０．１Ｍとなるよう
に、ｎ−ブタノール、酢酸および水の混液（３：１：１
．Ｖ／Ｖ）に溶解した。ヒスチジンは０．１Ｍとなるよ
うに水に溶解した。各液０．２１Ｌ文を６ 、７００人
又は１１，５００人の小孔を有する実施例１と同一の大
きさのポーラスガラスシートにスポットした。ｎ〜フッ
タール、酢酸と水の混液（３：１ ： １ 、 Ｖ／Ｖ
）て展開後、ガラスシートをドライヤーて乾燥し、ニ
ンヒドリンのメタノール溶液（０，２ｇ／ｌｏｏ 層
ｌ）をスプレーし、ドライヤーの熱風て乾燥させながら
呈色反応させた。[Example 4] Phenylalanine and alanine were mixed in a mixture of n-butanol, acetic acid and water (3:1:1) so that the concentration was 0.1M.
．． V/V). Histidine was dissolved in water to a concentration of 0.1M. 0.21 L of each solution was spotted onto a porous glass sheet of the same size as Example 1 having 6,700 or 11,500 holes. n ~ phthalate, acetic acid and water mixture (3:1:1, V/V
), the glass sheet was dried using a dryer, and a methanol solution of ninhydrin (0.2 g/loo layer 1) was sprayed on it, and a color reaction was caused while drying with hot air from a dryer.
各アミノ酸は紫色に呈色した。第５．６図は夫々ＩＩ、
５００人、 ６，７００人の小孔を有するシートを用い
た場合のクロマトグラムである。各アミノ酸は図に示す
ように、どちらのシートでもよく分離した。展開所要時
間は夫々２５ｍ１ｎ、２５ｍ１ｎであった。Each amino acid was colored purple. Figure 5.6 shows II, respectively.
This is a chromatogram when using sheets with 500 and 6,700 pores. As shown in the figure, each amino acid was well separated on both sheets. The time required for development was 25 m1n and 25 m1n, respectively.
［発明の効果］
試料の展開、分離を短時間で精度よく行うことかでき、
又分離された成分の同定、定量を強い反応性を有する検
出試薬を用い、或は高温で行うことが可能となる。[Effects of the invention] Sample development and separation can be carried out in a short time and with high precision.
Furthermore, it becomes possible to identify and quantify the separated components using a highly reactive detection reagent or at high temperatures.
又分離された各成分の付着したシートの所定部分を切取
り、次工程に利用することが可能となる。Furthermore, it is possible to cut out a predetermined portion of the sheet to which each separated component has adhered and use it in the next step.
第１〜６図は本発明の薄層クロマトグラフィーシートを
用いて得られたクロマトグラムである。
第１図
箭４図1 to 6 are chromatograms obtained using the thin layer chromatography sheet of the present invention. Figure 1: Illustration 4
Claims (1)
薄層クロマトグラフィーシート。（２）多孔質ガラスは
ＳｉＯ＿２４５〜７０ｗｔ％、Ｂ＿２Ｏ＿３８〜３０ｗ
ｔ％、ＣａＯ８〜２５ｗｔ％、Ａｌ＿２Ｏ＿３５〜１５
ｗｔ％、Ｎａ＿２Ｏ３〜８ｗｔ％、Ｋ＿２Ｏ１〜５ｗｔ
％、Ｎａ＿２Ｏ＋ｋ＿２Ｏ４〜１３ｗｔ％、ＭｇＯ０〜
８ｗｔ％、又はＳｉＯ＿２４５〜７０ｗｔ％、Ｂ＿２Ｏ
＿３８〜３０ｗｔ％、ＣａＯ８〜２５ｗｔ％、Ａｌ＿２
Ｏ＿３５〜１５ｗｔ％なる組成を有するガラスを熱処理
してＢ＿２Ｏ＿３、ＣａＯを主体とする相を分相せしめ
、この相を溶解除去することによって得られるものであ
る請求項１記載の薄層クロマトグラフィーシート。 （３）多孔質ガラスの孔径は１，０００〜１２，０００
Åである請求項２記載の薄層クロマトグラフィーシート
。 （４）ＳｉＯ＿２４５〜７０ｗｔ％、Ｂ＿２Ｏ＿３８〜
３０ｗｔ％、ＣａＯ８〜２５ｗｔ％、Ａｌ＿２Ｏ＿３５
〜１５ｗｔ％、Ｎａ＿２Ｏ３〜８ｗｔ％、Ｋ＿２Ｏ１〜
５ｗｔ％、Ｎａ＿２Ｏ＋Ｋ＿２Ｏ４〜１３ｗｔ％、Ｍｇ
Ｏ０〜８ｗｔ％、又はＳｉＯ＿２４５〜７０ｗｔ％、Ｂ
＿２Ｏ＿３８〜３０ｗｔ％、ＣａＯ８〜２５ｗｔ％、Ａ
ｌ＿２Ｏ＿３５〜１５ｗｔ％なる組成を有するガラス成
形体を熱処理してＢ＿２Ｏ＿３、ＣａＯを主体とする相
を分相せしめ、この相を溶解除去することを特徴とする
薄層クロマトグラフィーシートの製造法。 （５）Ｂ＿２Ｏ＿３、ＣａＯ相の分相除去をＢ＿２Ｏ＿
３が残存する条件下に行なう請求項４記載の薄層クロマ
トグラフィーシートの製造法。 （６）Ｂ＿２Ｏ＿３の残存量が０．５ｗｔ％以上である
請求項５記載の薄層クロマトグラフィーシートの製造法
。[Scope of Claims] (1) A thin layer chromatography sheet made of a porous glass sheet having a large number of small pores. (2) Porous glass is SiO_245-70wt%, B_2O_38-30w
t%, CaO8~25wt%, Al_2O_35~15
wt%, Na_2O3~8wt%, K_2O1~5wt
%, Na_2O+k_2O4~13wt%, MgO0~
8wt%, or SiO_245-70wt%, B_2O
_38-30wt%, CaO8-25wt%, Al_2
2. The thin layer chromatography sheet according to claim 1, which is obtained by heat-treating a glass having a composition of O_35 to 15 wt% to separate a phase mainly composed of B_2O_3 and CaO, and dissolving and removing this phase. (3) The pore diameter of porous glass is 1,000 to 12,000
3. The thin layer chromatography sheet according to claim 2, which is . (4) SiO_245~70wt%, B_2O_38~
30wt%, CaO8-25wt%, Al_2O_35
~15wt%, Na_2O3~8wt%, K_2O1~
5wt%, Na_2O+K_2O4~13wt%, Mg
O0~8wt%, or SiO_245~70wt%, B
_2O_38-30wt%, CaO8-25wt%, A
A method for producing a thin layer chromatography sheet, which comprises heat-treating a glass molded body having a composition of 35 to 15 wt% l_2O_3 to separate a phase mainly composed of B_2O_3 and CaO, and dissolving and removing this phase. (5) B_2O_3, phase separation removal of CaO phase by B_2O_
5. The method for producing a thin layer chromatography sheet according to claim 4, wherein the method is carried out under conditions where 3 remains. (6) The method for producing a thin layer chromatography sheet according to claim 5, wherein the residual amount of B_2O_3 is 0.5 wt% or more.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16582888A JPH0216447A (en) | 1988-07-05 | 1988-07-05 | Thin-layer chromatography sheet and its production |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16582888A JPH0216447A (en) | 1988-07-05 | 1988-07-05 | Thin-layer chromatography sheet and its production |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0216447A true JPH0216447A (en) | 1990-01-19 |
Family
ID=15819775
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP16582888A Pending JPH0216447A (en) | 1988-07-05 | 1988-07-05 | Thin-layer chromatography sheet and its production |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0216447A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8256370B2 (en) | 2008-05-14 | 2012-09-04 | Tokyo Electron Limited | Coating apparatus and method |
| US8551563B2 (en) | 2008-05-13 | 2013-10-08 | Tokyo Electron Limited | Coating method |
-
1988
- 1988-07-05 JP JP16582888A patent/JPH0216447A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8551563B2 (en) | 2008-05-13 | 2013-10-08 | Tokyo Electron Limited | Coating method |
| US8256370B2 (en) | 2008-05-14 | 2012-09-04 | Tokyo Electron Limited | Coating apparatus and method |
| US8808798B2 (en) | 2008-05-14 | 2014-08-19 | Tokyo Electron Limited | Coating method |
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