JP2548874B2 - Chromatographic separation packing material - Google Patents
Chromatographic separation packing materialInfo
- Publication number
- JP2548874B2 JP2548874B2 JP4274504A JP27450492A JP2548874B2 JP 2548874 B2 JP2548874 B2 JP 2548874B2 JP 4274504 A JP4274504 A JP 4274504A JP 27450492 A JP27450492 A JP 27450492A JP 2548874 B2 JP2548874 B2 JP 2548874B2
- Authority
- JP
- Japan
- Prior art keywords
- silica gel
- packing material
- chromatographic separation
- separation
- gel particles
- 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 - Fee Related
Links
- 239000000463 material Substances 0.000 title claims description 16
- 238000012856 packing Methods 0.000 title claims description 15
- 238000013375 chromatographic separation Methods 0.000 title claims description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 41
- 239000000741 silica gel Substances 0.000 claims description 38
- 229910002027 silica gel Inorganic materials 0.000 claims description 38
- 239000002245 particle Substances 0.000 claims description 22
- 238000001035 drying Methods 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 2
- 159000000003 magnesium salts Chemical class 0.000 claims 1
- 238000000926 separation method Methods 0.000 description 17
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 10
- 239000011777 magnesium Substances 0.000 description 10
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 9
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 9
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 9
- 229910052749 magnesium Inorganic materials 0.000 description 9
- 150000007514 bases Chemical class 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- NIQCNGHVCWTJSM-UHFFFAOYSA-N Dimethyl phthalate Chemical compound COC(=O)C1=CC=CC=C1C(=O)OC NIQCNGHVCWTJSM-UHFFFAOYSA-N 0.000 description 6
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 6
- 238000004587 chromatography analysis Methods 0.000 description 5
- 238000004128 high performance liquid chromatography Methods 0.000 description 5
- 238000004305 normal phase HPLC Methods 0.000 description 5
- 238000001179 sorption measurement Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 4
- 150000002681 magnesium compounds Chemical class 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- FBSAITBEAPNWJG-UHFFFAOYSA-N dimethyl phthalate Natural products CC(=O)OC1=CC=CC=C1OC(C)=O FBSAITBEAPNWJG-UHFFFAOYSA-N 0.000 description 3
- 229960001826 dimethylphthalate Drugs 0.000 description 3
- 229910001629 magnesium chloride Inorganic materials 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 description 2
- 239000000395 magnesium oxide Substances 0.000 description 2
- -1 methanol Chemical compound 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 230000000274 adsorptive effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910052910 alkali metal silicate Inorganic materials 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 238000001479 atomic absorption spectroscopy Methods 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- HPYNZHMRTTWQTB-UHFFFAOYSA-N dimethylpyridine Natural products CC1=CC=CN=C1C HPYNZHMRTTWQTB-UHFFFAOYSA-N 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000011325 microbead Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000011002 quantification Methods 0.000 description 1
- 239000012266 salt solution Substances 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
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
Landscapes
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Treatment Of Liquids With Adsorbents In General (AREA)
Description
【０００１】[0001]
【産業上の利用分野】本発明は、クロマト分離用充填剤
に関するものであり、詳しくは、塩基性物質の吸着分離
が良好にできるシリカゲル粒子を母体とする充填剤に関
するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a packing material for chromatographic separation, and more particularly to a packing material having silica gel particles as a base material, which can favorably adsorb and separate a basic substance.
【０００２】[0002]
【従来技術】シリカゲル粒子を高速液体クロマトグラフ
ィーの充填剤として用いることは公知であり、一般的
に、このクロマトグラフィーは吸着（順相）クロマトグ
ラフィーとして各種溶質の分析又は精製の目的で広く利
用されている。この作用機構はシリカゲル表面との溶質
との相互作用が基本となるが、シリカゲルの表面シラノ
ール（Ｓｉ−ＯＨ）基による溶質との水素結合性が主で
あると言われている。BACKGROUND OF THE INVENTION It is known to use silica gel particles as a packing material for high performance liquid chromatography, and this chromatography is generally used as adsorption (normal phase) chromatography for the purpose of analyzing or purifying various solutes. ing. This action mechanism is basically based on the interaction with the solute on the surface of silica gel, but it is said that the hydrogen bonding property with the solute by the surface silanol (Si-OH) group of silica gel is the main.
【０００３】しかしながら、表面シラノール基は解離し
て酸性状態となりイオン交換的な作用を示す場合もあ
り、特に、溶質が塩基性物質の場合には、シリカとイオ
ン結合を生成するため異常に強い吸着を示し、その結
果、塩基性物質に対するクロマトグラフィーの吸着分離
が良好に行なわれないとの欠点があった。However, the surface silanol group may be dissociated to be in an acidic state and exhibit an ion-exchange-like action. Especially, when the solute is a basic substance, it forms an ionic bond with silica, resulting in abnormally strong adsorption. As a result, there was a drawback that the adsorption separation of the basic substance by chromatography could not be performed well.
【０００４】[0004]
【発明が解決しようとする課題】本発明は上記実情に鑑
み、シリカゲル粒子を充填剤とした場合のクロマト分離
技術において、塩基性化合物の吸着分離を容易に確実に
行なうための方法を提供しようとするものである。In view of the above situation, the present invention intends to provide a method for easily and surely performing adsorption separation of a basic compound in a chromatographic separation technique using silica gel particles as a packing material. To do.
【０００５】[0005]
【課題を解決するための手段】本発明者等は上記の目的
を達成すべく種々検討を重ねた結果、クロマト分離用の
充填剤として用いるシリカゲル粒子をマグネシウム化合
物で処理した場合には、溶質中に塩基性化合物を含んで
いても該化合物の吸着分離が良好にできることを見い出
し本発明を完成した。Means for Solving the Problems The present inventors have conducted various studies to achieve the above object, and as a result, when silica gel particles used as a packing material for chromatographic separation were treated with a magnesium compound, The present invention has been completed by finding that even if a basic compound is contained in the compound, the compound can be favorably adsorbed and separated.
【０００６】すなわち、本発明の要旨は、マグネシウム
塩の水溶液中にシリカゲルを浸漬しｐＨ５．５以上に調
整保持した後、これを分離、乾燥することにより得たシ
リカゲル粒子よりなることを特徴とするクロマト分離用
充填剤に存する。以下、本発明の構成につき詳細に説明
する。本発明において対象となるシリカゲル粒子として
は、特に限定されるものではなく、従来からクロマトグ
ラフィー用充填剤として公知のものでよく、通常、ケイ
酸アルカリの中和反応により得られる平均粒径３〜５０
０μｍの球状及び破砕状シリカゲルが挙げられる。ま
た、シリカゲル粒子の物性値としては、例えば、細孔容
積が０．２〜２．０ｍｌ／ｇ、比表面積が１０〜８００
ｍ2 ／ｇであり、更に平均細孔径が１００００オングス
トローム以下のものが好適に挙げられる。That is, the gist of the present invention is magnesium
Adjust the pH to 5.5 or higher by immersing the silica gel in the salt solution.
A packing material for chromatographic separation, which comprises silica gel particles obtained by isolating and drying the silica gel after the preparation and holding. Hereinafter, the configuration of the present invention will be described in detail. The silica gel particles to be used in the present invention are not particularly limited and may be those conventionally known as a packing material for chromatography, and usually have an average particle size of 3 to 3 obtained by a neutralization reaction of alkali silicate. Fifty
Examples include 0 μm spherical and crushed silica gel. The physical properties of silica gel particles include, for example, a pore volume of 0.2 to 2.0 ml / g and a specific surface area of 10 to 800.
Preferred are those having m 2 / g and further having an average pore diameter of 10,000 angstroms or less.
【０００７】本発明においては、上記シリカゲル粒子を
予めマグネシウム化合物の水溶液により処理したものを
充填剤として用いるが、マグネシウム化合物としては、
例えば、塩化マグネシウム、硝酸マグネシウムなど水溶
性のマグネシウム化合物が挙げられ、なかでも塩化マグ
ネシウムが特に好ましい。マグネシウム溶液のｐＨ値が
低いとシリカゲル粒子へのマグネシウムの結合が効率的
に行なわれないので、通常、水溶液ｐＨが５．５以上、
好ましくは６〜１０となるような濃度に水酸化ナトリウ
ム、水酸化カルシウム、アンモニア水等のアルカリを加
えて調節するのが望ましい。特にアンモニア水は処理後
乾燥により容易に除去できるので望ましい。このｐＨに
よって最終的に得られるシリカゲル中のマグネシウム含
有量をコントロールすることができる。In the present invention, the silica gel particles previously treated with an aqueous solution of a magnesium compound are used as the filler.
Examples thereof include water-soluble magnesium compounds such as magnesium chloride and magnesium nitrate, and magnesium chloride is particularly preferable. If the pH value of the magnesium solution is low, the binding of magnesium to the silica gel particles is not performed efficiently, so normally the pH of the aqueous solution is 5.5 or more,
It is desirable to adjust the concentration by adding an alkali such as sodium hydroxide, calcium hydroxide or aqueous ammonia to a concentration of preferably 6 to 10. In particular, ammonia water is desirable because it can be easily removed by drying after the treatment. The pH can control the magnesium content in the finally obtained silica gel.
【０００８】シリカゲル粒子とマグネシウム化合物水溶
液との接触処理は、通常、前記水溶液中にシリカゲル粒
子を浸漬させることにより行なうことができる。この際
の処理温度は、通常、５〜５０℃程度であり、また、処
理時間は５〜１２０分程度である。なお、この接触処理
をシリカゲルの充填層に前記水溶液を通水する充填塔形
式で実施することもできる。接触処理後のシリカゲル粒
子は必要に応じて、水及び／又はメタノールなどのアル
コールなどで洗浄した後、乾燥処理される。乾燥温度は
通常、１００〜１５０℃程度であり、この乾燥によって
通常、マグネシウムはマグネシアとなってシリカゲル粒
子表面に結合する。乾燥後更に４００℃以上、好ましく
は５５０℃以上で焼成しても良い。The contact treatment between the silica gel particles and the magnesium compound aqueous solution can usually be carried out by immersing the silica gel particles in the aqueous solution. The treatment temperature at this time is usually about 5 to 50 ° C., and the treatment time is about 5 to 120 minutes. Note that this contact treatment can also be carried out in the form of a packed tower in which the aqueous solution is passed through a packed bed of silica gel. The silica gel particles after the contact treatment are, if necessary, washed with water and / or alcohol such as methanol, and then dried. The drying temperature is usually about 100 to 150 ° C., and this drying usually causes magnesium to become magnesia and bond to the surface of the silica gel particles. After drying, it may be further baked at 400 ° C. or higher, preferably 550 ° C. or higher.
【０００９】このようにしてマグネシウム成分がコート
された本発明のシリカゲル粒子を得ることができる。こ
こで得た本発明のシリカゲル粒子は塩基性物質とのイオ
ン交換的結合を抑えることができるので、これをクロマ
ト分離用充填剤として使用した場合の塩基性化合物の分
離を良好に行なうことができる。焼成したものは共存す
る酸性物質も分離することができる。シリカゲル粒子へ
のマグネシウム含有量は本発明の目的を達成する上では
高いほど望ましいが、通常、処理後のシリカゲル粒子の
ｐＨ（５％水スラリーとした場合の水相のｐＨ）が７．
０以上、好ましくは７．５以上を示すような量が好まし
い。また、シリカ粒子のマグネシウム含有量が、通常、
２００ｐｐｍ以上、好ましくは５００〜５０００ｐｐｍ
のものが好ましい。Thus, the silica gel particles of the present invention coated with the magnesium component can be obtained. Since the silica gel particles of the present invention obtained here can suppress the ion exchange bond with the basic substance, when the silica gel particles are used as a packing material for chromatographic separation, the basic compound can be well separated. . The calcined product can also separate coexisting acidic substances. The magnesium content in the silica gel particles is preferably as high as possible in order to achieve the object of the present invention, but usually the pH of the silica gel particles after the treatment (pH of the aqueous phase in the case of 5% water slurry) is 7.
The amount is preferably 0 or more, and more preferably 7.5 or more. The magnesium content of the silica particles is usually
200 ppm or more, preferably 500 to 5000 ppm
Are preferred.
【００１０】本発明のクロマト分離用充填剤は常法に従
って、例えば、高速液体クロマトグラフィーの充填剤ま
たはその他クロマト分離用の充填剤として用いることが
できる。そして、各種化合物の分析又は分離、精製に適
用することができる。特に、本発明の充填剤は例えば、
アミン類などの塩基性化合物に対しても有効な吸着分離
をすることができ、複数のアミン類を含む溶質の高精度
分析又は効率的分離、精製が可能となる。The packing material for chromatographic separation of the present invention can be used according to a conventional method, for example, as a packing material for high performance liquid chromatography or other packing material for chromatographic separation. Then, it can be applied to analysis or separation and purification of various compounds. In particular, the filler of the present invention is, for example,
It is possible to perform effective adsorptive separation even for basic compounds such as amines, and it is possible to perform highly accurate analysis or efficient separation and purification of a solute containing a plurality of amines.
【００１１】[0011]
【実施例】次に、本発明を実施例を更に具体的に説明す
るが、本発明はその要旨を超えない限り、以下の実施例
の記述に制約されるものではない。 実施例１、２、３ ［製法］ＨＰＬＣ用シリカゲル（スーパーマイクロビー
ズ １００オングストローム、１０μｍ）１０ｇを塩化
マグネシウム（ＭｇＣｌ2 ・６Ｈ2 Ｏ）２．５ｇを加え
た蒸留水１００ｍｌ中に浸漬し、このスラリーを室温で
攪拌しながら６Ｎアンモニウム水をゆっくり加え表１に
示すｐＨに調整し、その後３０分間保持した後、吸引濾
過しシリカゲルを回収した。次いで，各々回収したシリ
カゲルを蒸留水１００ｍｌとメタノール１００ｍｌで順
次洗浄した後、１１０℃の温度で乾燥処理することによ
り本発明のシリカゲルを得た。EXAMPLES Next, the present invention will be described in more detail with reference to examples, but the present invention is not limited to the description of the following examples as long as the gist thereof is not exceeded. Examples 1, 2, 3 [Production Method] 10 g of silica gel for HPLC (Super Microbeads 100 angstrom, 10 μm) was immersed in 100 ml of distilled water to which 2.5 g of magnesium chloride (MgCl 2 .6H 2 O) was added, and this slurry was prepared. While stirring at room temperature, 6N ammonium water was slowly added to adjust the pH to the value shown in Table 1, and after holding it for 30 minutes, suction filtration was performed to collect silica gel. Next, the recovered silica gel was washed successively with 100 ml of distilled water and 100 ml of methanol and then dried at a temperature of 110 ° C. to obtain the silica gel of the present invention.
【００１２】ここで得られた各球状シリカゲルについ
て、Ｍｇ含有量（フッ酸処理−原子吸光法により定量）
及び５％水スラリーとした場合のｐＨなどの物性値を測
定した結果を表１に示す。 実施例４ 侵漬時のｐＨを９．０として保持し、乾燥処理後６００
℃で２時間焼成する以外は実施例１と同様にしてシリカ
ゲルを得た。For each spherical silica gel obtained here, the Mg content (hydrofluoric acid treatment-quantification by atomic absorption spectrometry)
Table 1 shows the results of measurement of physical properties such as pH in the case of using 5% water slurry. Example 4 The pH at the time of immersion was maintained at 9.0, and after the drying treatment, 600
Silica gel was obtained in the same manner as in Example 1 except that calcination was performed for 2 hours.
【００１３】[0013]
【表１】 [Table 1]
【００１４】［クロマト分離テスト］上記処理により得
られた各球状シリカゲルを充填した高速液体クロマトグ
ラフィーカラムを用い、ベンゼン、フタル酸ジメチル及
びピリジンよりなる試料について下記条件で順相高速液
体クロマト分離特性の試験を行なったところ、図１〜
３、５に示すような各ピークが得られ、ピーク１がベン
ゼン、ピーク２がフタル酸ジメチル、ピーク３がピリジ
ン、ピーク４がフェノールであり、各成分の吸着分離を
良好に行なうことができた。[Chromatographic Separation Test] Using a high performance liquid chromatography column packed with each spherical silica gel obtained by the above-mentioned treatment, a sample consisting of benzene, dimethyl phthalate and pyridine was tested for normal phase high performance liquid chromatography separation characteristics under the following conditions. When the test was conducted,
The respective peaks as shown in 3 and 5 were obtained, and the peak 1 was benzene, the peak 2 was dimethyl phthalate, the peak 3 was pyridine, and the peak 4 was phenol. .
【００１５】カラム：４．６φ×２５０mm（ステンレス
製） 移動相：１％メタノール／ｎ−ヘキサン 流速 ：１ｍｌ／min 検出 ：ＵＶ２５４nm なお、ピリジンのＫ´値、理論段数、対称性を求めた結
果を表２に示す。Column: 4.6φ × 250 mm (stainless steel) Mobile phase: 1% methanol / n-hexane Flow rate: 1 ml / min Detection: UV254 nm The K ′ value of pyridine, the number of theoretical plates, and the symmetry were obtained. It shows in Table 2.
【００１６】[0016]
【表２】 [Table 2]
【００１７】比較例１ 実施例１において、マグネシウム処理をしていない球状
シリカゲルを充填した高速液体クロマトグラフィーカラ
ムを用いて同様の試料について同条件で順相高速液体ク
ロマト分離特性の試験をしたところ、図４に示すピーク
が得られ、ピーーク３すなわちピリジンが溶出していな
い。Comparative Example 1 In Example 1, the same sample was tested for normal phase high performance liquid chromatographic separation characteristics under the same conditions using a high performance liquid chromatography column packed with non-magnesium treated spherical silica gel. The peak shown in FIG. 4 was obtained, and peak 3 or pyridine was not eluted.
【００１８】[0018]
【発明の効果】本発明のクロマトグラフィー用充填剤に
よれば、シリカゲル粒子の表面がマグネシアによってコ
ートされているためか、たとえ溶質中に塩基性化合物を
含んでいても、これら塩基性化合物の吸着分離を良好に
行なうことができる。従って、塩基性化合物に対して精
度の高いの分析が可能となり、また、より効率の良い分
離精製を実現することができる。According to the packing material for chromatography of the present invention, the surface of silica gel particles is coated with magnesia. Even if the solute contains a basic compound, the adsorption of these basic compounds The separation can be performed well. Therefore, it is possible to analyze a basic compound with high accuracy, and it is possible to realize more efficient separation and purification.
【図１】 実施例１の順相高速液体クロマト分離特性試
験における分離ピークを示す。1 shows separation peaks in a normal phase high performance liquid chromatographic separation characteristic test of Example 1. FIG.
【図２】 実施例２の順相高速液体クロマト分離特性試
験における分離ピークを示す。FIG. 2 shows separation peaks in a normal phase high performance liquid chromatography separation characteristic test of Example 2.
【図３】 実施例３の順相高速液体クロマト分離特性試
験における分離ピークを示す。FIG. 3 shows separation peaks in a normal phase high performance liquid chromatography separation characteristic test of Example 3.
【図４】 比較例１の順相高速液体クロマト分離特性試
験における分離ピークを示す。FIG. 4 shows separation peaks in a normal phase high performance liquid chromatography separation characteristic test of Comparative Example 1.
【図５】 実施例４の順相高速液体クロマト分離特性試
験における分離ピークを示す。FIG. 5 shows separation peaks in a normal phase high performance liquid chromatography separation characteristic test of Example 4.
１…ベンゼン，２…フタル酸ジメチル，３…ピリジン，
４…フェノール1 ... benzene, 2 ... dimethyl phthalate, 3 ... pyridine,
4 ... phenol
Claims (2)
を浸漬しｐＨ５．５以上に調整保持した後、これを分
離、乾燥することにより得たシリカゲル粒子よりなるこ
とを特徴とするクロマト分離用充填剤。1. A packing material for chromatographic separation, characterized by comprising silica gel particles obtained by immersing silica gel in an aqueous solution of magnesium salt, adjusting and maintaining the pH to 5.5 or more, separating and drying the silica gel.
カゲル粒子よりなる請求項１記載のクロマト分離用充填
剤。2. The packing material for chromatographic separation according to claim 1, which comprises silica gel particles obtained by further drying and then calcining.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4274504A JP2548874B2 (en) | 1992-10-13 | 1992-10-13 | Chromatographic separation packing material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4274504A JP2548874B2 (en) | 1992-10-13 | 1992-10-13 | Chromatographic separation packing material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH06123734A JPH06123734A (en) | 1994-05-06 |
| JP2548874B2 true JP2548874B2 (en) | 1996-10-30 |
Family
ID=17542620
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP4274504A Expired - Fee Related JP2548874B2 (en) | 1992-10-13 | 1992-10-13 | Chromatographic separation packing material |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2548874B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010203794A (en) * | 2009-02-27 | 2010-09-16 | Fuji Silysia Chemical Ltd | Method of separating acidic organic compound |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5245239B2 (en) * | 1972-06-15 | 1977-11-14 | ||
| JPS52107290A (en) * | 1975-09-30 | 1977-09-08 | Shimadzu Corp | Method and apparatus for producing diatomaceous earth carrier |
-
1992
- 1992-10-13 JP JP4274504A patent/JP2548874B2/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010203794A (en) * | 2009-02-27 | 2010-09-16 | Fuji Silysia Chemical Ltd | Method of separating acidic organic compound |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH06123734A (en) | 1994-05-06 |
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