JPH0711516B2 - Chromatogram concentration / transfer method - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION (Industrial field of application) The present invention relates to thin layer chromatography (TLC) and paper chromatography, and to thin layer chromatography plates and paper chromatography papers (these are collectively referred to as thin layer plates). The present invention relates to a method for concentrating the developed fraction and transferring it to a medium convenient for analysis by infrared spectroscopy.

(Prior Art) As a plate used in thin layer chromatography, a plate obtained by coating silica gel on a glass substrate or an aluminum sheet is generally used. In paper chromatography, filter paper is used.

FIG. 3 shows a cross section of a conventional thin layer chromatography plate. 2 is a glass substrate or an aluminum sheet, and a silica gel layer 4 is formed on the surface thereof. The sample is spread in the in-plane direction of the silica gel layer 4 by the eluent to form the fraction 6.

The sample fraction developed on the thin layer plate is directly measured with a densitometer, or the fraction is scraped, extracted, concentrated, and then spectroscopically measured.

Attempts have also been made to analyze the components developed on thin-layer plates by Fourier transform infrared spectroscopy (FTIR). To analyze by FTIR, the developed fraction is directly squeezed with infrared light and the diffuse reflectance spectrum is measured (see Anal. Chem. 1989 , 61, 615-618). , KBr and KCl powder pellets, dried and measured by FTIR (Anal. Chem. 19
87 , 59, 415-418), placing a powder without infrared absorption on the edge of a thin plate and transferring the fractional component from the thin plate to the powder through glass fiber (Anal.C.
hem. 1986, and references 58,2708-2714) has been attempted.

(Problems to be Solved by the Invention) A method of scraping, extracting and concentrating a fraction for performing spectroscopic measurement is inaccurate and troublesome.

The method of directly irradiating the thin plate with infrared rays for FTIR measurement is not practical because the infrared absorption of silica gel or paper of the thin layer plate is large.

The method of scraping and extracting the component fractions and dropping them on KBr or KCl powder pellets for FTIR measurement is inaccurate and cumbersome.

In the method of transferring the fractional component by using the glass fiber at the edge of the thin plate, the resolution in the developing direction is determined by the pitch of the glass fiber provided at the edge, and only the thin plate that is one-dimensionally developed can be used. Not applicable.

It is an object of the present invention to enable accurate and simple measurement by a densitometer and spectroscopic measurement by directly concentrating on a thin layer plate.

The present invention also, when performing infrared spectroscopic analysis of the fraction component, without scraping the fraction, by directly transferring the fraction developed on the thin layer plate to the infrared reflective material layer,
The purpose is to enable accurate infrared spectroscopic analysis.

(Means for Solving the Problems) In the concentration method of the present invention, a thin layer plate having a sample fraction and no support material is placed on a porous material plate, and an eluent is directed from the porous material plate to the thin layer plate. Rises by capillarity,
The fractionated sample in the thin layer plate is concentrated on the surface by volatilizing from the surface of the thin layer plate.

In the transfer method of the present invention, a thin layer plate having a sample fraction and no support material is placed on a porous material plate, an infrared reflecting material layer is brought into close contact with the thin layer plate, and an eluent is added to the porous material plate. From the surface through the thin layer plate toward the infrared reflecting material layer by a capillary phenomenon, and volatilized from the surface of the infrared reflecting material layer to transfer the fractionated sample in the thin layer plate to the infrared reflecting material layer.

(Function) The sample is developed and separated using a thin layer plate that does not use a supporting material, and the eluent is moved from one surface of the thin layer plate to the other surface by capillarity so that the separated component is separated from the other surface. Can be concentrated to.

In addition, the infrared reflective material layer is adhered to one surface of the thin layer plate from which the sample has been developed and separated, and the eluent from the other side of the thin layer plate is moved to the side having the infrared reflective material layer by capillary action. By moving, the separation component can be moved and transferred in the direction of the infrared reflective material layer.

(Example) FIG. 1 shows an example showing the concentration method of the present invention.

A porous substrate 10 is placed in the container 8, and a membrane layer plate 12 on which a sample is spread is placed on the porous substrate 10. The thin layer plate 12 is a thin layer chromatography plate and does not use a support material. Empore TLC sheet (Analytichem Internatio
nal, Inc.) or a glass sintered plate can be used. The thin layer plate 12 may also be a paper for paper chromatography. The thin plate 12 has the sample already developed and the fractions are present. As the porous substrate 10, for example, a ceramic substrate or a material having a solution-permeable property such as paper or cloth is used.

The container 8 is filled with the eluent 14 until a part of the porous substrate 10 is immersed.
Put in. Although various solvents can be used as the eluent 14, chloroform is used, for example.

In this state, the eluent 14 moves to the surface side through the porous substrate 10 by a capillary phenomenon, and the sample fraction developed on the thin layer plate 12 is concentrated on the surface side of the thin layer plate 12. 16 is a concentrated sample fraction.

At this time, in order to promote the volatilization of the eluent that has reached the surface of the thin layer plate 12, if air is blown, the concentration can be performed more quickly.

FIG. 2 shows an embodiment in which the fractional components of the thin layer plate 12 are transferred to the infrared reflecting material layer.

In the container 8, two porous substrates 10a and 10b are placed in an overlapping manner. The upper porous substrate 10b can be removed from the lower porous substrate 10a. On the upper porous substrate 10b, a thin layer plate 12 without a supporting material is placed. The thin plate 12 may be a thin plate as described in FIG. 1, for example Empore T
It is an LC sheet, a glass sintered plate, or paper for paper chromatography.

An infrared reflecting material layer 18 is further formed on the thin plate 12 in close contact with it. As the infrared reflective material layer 18, KBr or K
A powdered material of an infrared reflective material such as Cl or a plate-shaped material such as an alumina ceramic plate is used. An infrared reflecting material layer 18 is formed on the thin layer plate 12 in a state where the sample is spread in the thin layer plate 12 and a fraction exists.
When the infrared reflective material layer 18 is formed as a powder layer, when the thin plate 12 is a flexible material such as an EmporeTLC sheet, the powder layer formed on the surface thereof is fragile, so that the porous substrate 10b is formed. The thin layer plate 12 is placed on the thin layer plate 12, the powder layer 18 is formed on the thin layer plate 12, and then the porous substrate 10b is placed on the porous substrate 10a.

The eluent 14 is added to such an extent that a part of the lower porous substrate 10a is immersed.

In this state, the eluent 14 passes through the porous substrates 10a and 10b, rises in the thin plate 12 to reach the infrared reflective material layer 18, and is evaporated from the surface of the infrared reflective material layer 18. At this time, the sample component in the thin layer plate 12 moves upward as the eluent 14 moves, and is transferred to the infrared reflective material layer 18. Reference numeral 20 is a transferred sample component.

Also in the case of FIG. 2, it is effective to blow air in order to accelerate the volatilization of the eluent from the surface of the infrared reflective material layer 18.

(Effects of the Invention) In the present invention, since the fractionated sample is concentrated on the surface side of the thin layer plate by moving the eluent in the thickness direction of the thin layer plate without using the support material, the densitometer The measurement and the spectroscopic measurement can be performed accurately, and the concentration operation is simple.

In the case of performing infrared spectroscopic analysis, an infrared reflecting material layer is provided in close contact with a thin layer plate having no supporting material, and the eluent is moved from the lower side of the thin layer plate toward the infrared reflecting material layer. As a result, since the fractionated sample component is transferred to the infrared reflective material layer, accurate infrared spectroscopic analysis can be performed, and the transfer operation is simple.

[Brief description of drawings]

FIG. 1 is a sectional view of an embodiment showing the concentration method of the present invention, and FIG. 2 is a sectional view of an embodiment showing the transfer method of the present invention.
The figure is a cross-sectional view showing a thin layer plate for ordinary thin layer chromatography. 10,10a, 10b ... Porous substrate, 12 ... Thin layer plate, 16 ...
… Concentrated fraction components, 18 …… Infrared reflective material layer, 20 ……
The transferred fractional component.

 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Tomiyuki Maeda, No. 1 Nishinokyo Kuwabara-cho, Nakagyo-ku, Kyoto City, Kyoto Prefecture Shimazu Corporation Sanjo Factory (72) Inventor Takahiro Tajima Nishinokyo-Kuwabara-cho, Nakagyo-ku, Kyoto Prefecture Kyoto Stock Shimadzu Corporation Sanjo Factory (56) Reference JP-A-2-161351 (JP, A)

Claims (2)

[Claims] 1. A thin plate which has a sample fraction and does not use a supporting material is placed on a porous material plate, and the eluent is raised by capillary action from the porous material plate toward the thin layer plate to obtain a thin plate surface. A concentration method in which the fractionated sample in the thin layer plate is concentrated on the surface by volatilizing from the above. 2. A thin layer plate having a sample fraction and no support material is placed on a porous material plate, an infrared reflecting material layer is adhered to the thin layer plate, and the eluent is diluted from the porous material plate. A transfer method in which a fractional sample in a thin layer plate is transferred to the infrared reflective material layer by elevating by capillary action toward the infrared reflective material layer through the layer plate and volatilized from the surface of the infrared reflective material layer.