JP3838711B2 - Liquid chromatograph - Google Patents

Description

【００２３】
表１において、圧力上昇が早ければ早いほどフィルターＦ１の寿命が短いことを示すものである。従って、表１より、実施例１のクロマトグラフでは、フィルターＦを効果的に洗浄でき寿命が延びることに加え、フィルターＦ１の寿命も延びることが分かった。
【００２４】
【発明の効果】
本発明の液体クロマトグラフの構成は、上記の通りであり、試料注入のためのインジェクションバルブと試料吸引ノズルの間の流路に、フィルターが設置されているので、試料が流れる方向と逆方向に洗浄液を流すことにより、フィルターの洗浄を行うことができ、フィルターの詰まりを効果的に除去できるため、フィルターの長寿命化が図られ、かつ、分離性能を低下させない液体クロマトグラフを提供する。また、通常の液体クロマトグラフィー用自動試料導入装置には、逆洗浄のための装置が具備されているので、本発明の液体クロマトグラフは、従来の液体クロマトグラフ装置を僅かに改良するだけで製造できる。
【図面の簡単な説明】
【図１】本発明の液体クロマトグラフの構成を示す図である。
【図２】試料吸入時の、インジェクションバルブの接続状態を示す図である。
【図３】カラムに試料の注入時の、インジェクションバルブの接続状態を示す図である。
【図４】従来の液体クロマトグラフの構成を示す図である。
【符号の説明】
１ 移動相容器
２ 送液ポンプ
３ 試料導入装置
４ カラム
５ 検出器
６ インジェクションバルブ
７ 吸引器
８ 試料吸入ノズル
９ 試料容器
１１ 移動相
Ｆ フィルター
Ｆ１、Ｆ２、Ｆ３ フィルター
ａ、ｂ、ｃ、ｄ、ｅ、ｆ 接続口[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a liquid chromatograph.
[0002]
[Prior art]
Liquid chromatographs are widely used for separation and fractionation of components in samples in fields such as organic chemistry, biochemistry, and medicine. This liquid chromatograph is usually composed of an apparatus as shown in FIG. That is, it comprises a mobile phase container 1 in which a mobile phase such as an eluent is accommodated, a liquid feed pump 2 for feeding the mobile phase, a sample introduction device 3, a separation column 4 and a detector 5. The sample introduction device 3 is usually composed of an injection valve 6 comprising a six-way valve, a suction device 7, a sample suction nozzle 8, and a sample container 9.
[0003]
In order to separate a sample using the liquid chromatograph, a mobile phase 11 such as an eluent enters the separation column 4 via the sample introduction device 3 by the liquid feed pump 2, and the sample is separated by the separation column 4. Each component in it is separated. Each separated component is detected by the detector 5, for example, by measuring absorbance, and the result is expressed as a chromatogram (not shown).
[0004]
The liquid chromatograph is usually provided with a filter in its flow path so that insoluble matters in the sample and the eluent can be removed. Examples of such filter installation include the following.
(1) The filter F1 installed in the flow path between the injection valve 6 and the column 4 In this case, the purpose is mainly to remove insoluble matters derived from the sample introduced from the injection valve 6.
(2) Filter F2 installed in the flow path between the liquid feed pump 2 and the injection valve 6: In this case, the purpose is mainly to remove the wear and the like coming out of the plunger of the liquid feed pump 2.
(3) Filter F3 installed at the tip of the mobile phase suction nozzle: In this case, the purpose is mainly to remove dust and the like mixed in the mobile phase.
[0005]
These filters are used singly or in combination. However, any filter has a life span and needs to be replaced if the pressure increases due to clogging. However, the liquid chromatograph filter is expensive and its replacement work is troublesome. For this reason, it has been studied to extend the life of the filter. With regard to extending the life of the filter, for example, Japanese Patent Application Laid-Open No. 2-262504 discloses a filter in which the pore diameter of the filter sequentially changes in the flow direction of the eluent. However, this filter is complicated to manufacture and expensive. In addition, this filter has a problem that liquid is always allowed to flow only from one direction, so that it is difficult to remove what is clogged in the filter.
[0006]
Further, in the filter F1 installed in the flow path between the injection valve 6 and the column 4, there is a problem that the sample to be measured is diffused in the filter section and the separation performance is lowered.
[0007]
[Problems to be solved by the invention]
The present invention has been made in view of the above problems, and an object of the present invention is to provide a liquid chromatograph in which the life of the filter is extended and the separation performance is not deteriorated.
[0008]
[Means for Solving the Problems]
In the liquid chromatograph of the present invention, a filter is installed in the flow path between the injection valve for sample injection and the sample suction nozzle, and the injection valve, the sample suction nozzle, and the filter are measured with the same cleaning liquid. It has a mechanism for cleaning inside .
[0009]
The liquid chromatograph of the present invention will be described with reference to FIG. In the liquid chromatograph of the present invention, a filter F is installed in the flow path between the injection valve 6 for sample injection and the sample suction nozzle 8. The liquid chromatograph of the present invention is the same as the conventional liquid chromatograph of FIG. 4 because it is composed of the same device as the conventional liquid chromatograph except that the filter F is installed at the above position. The apparatus is given the same reference number, and the description thereof is omitted.
[0010]
As the filter used in the present invention, a known filter conventionally used in a liquid chromatograph can be used. As a material, a sintered body of a metal such as stainless steel; a ceramic; a synthetic polymer such as a fluororesin Etc.
[0011]
There is no restriction | limiting in particular as a shape of the said filter, A well-known shape may be sufficient, for example, disk shape, a column shape, etc. are mentioned.
[0012]
The method for installing the filter is the same as the known method, and the filter main body is housed in the holder and installed in the flow path.
[0013]
In the chromatograph of the present invention, in addition to the above-described filter F, the above-described filters F1, F2, and F3 that have been used conventionally may be installed. In this case, the durability of the column of the liquid chromatograph The property is further improved.
[0014]
[Action]
In the liquid chromatograph of the present invention, at the time of sample inhalation, as shown in FIG. 2, the connection ports a and b, c and d of the injection valve 6 are connected within the valve, and the aspirator 7 The sample is aspirated and filtered through filter F, and the sample is stored between loops bc. On the other hand, the connection ports e and f of the injection valve 6 are connected in the valve at this time, the mobile phase flows through the column, and the sample injected into the column is separated.
[0015]
When the sample is injected into the column, as shown in FIG. 3, the connection ports e and b, c and f of the injection valve 6 are connected in the valve, and the sample is stored between the loops bc. Is injected into the column. On the other hand, since the connection ports a and d of the injection valve 6 are connected in the valve at this time, the cleaning of the filter F is performed by flowing a cleaning liquid (not shown) from the suction device 7 side toward the filter F side. Can be performed. The cleaning liquid after cleaning the filter F is sent to a waste liquid container (not shown).
[0016]
As described above, in the chromatograph of the present invention, the filter can be cleaned by flowing the cleaning liquid in the direction opposite to the direction in which the sample flows. Is extended.
[0017]
In addition, since it is not necessary to install a filter in the flow path between the injection valve and the column, there is no reduction in separation performance due to diffusion of the sample to be measured in the filter section.
[0018]
DETAILED DESCRIPTION OF THE INVENTION
Hereinafter, the present invention will be described in detail by giving examples and comparative examples of the present invention.
[0019]
Example 1
The liquid chromatograph shown in FIG. 1 was assembled using the following apparatus.
Mobile phase container 1
Liquid feed pump 2: LC-9A, manufactured by Shimadzu Corporation
Sample introduction device 3: Automatic sample introduction using an automatic sample introduction device (SSU-420, manufactured by Sekisui Chemical Co., Ltd.) comprising an injection valve 6 comprising a hexagonal valve, a suction device 7, a sample suction nozzle 8 and a sample container 9. A filter F (a stainless sintered filter having a hole diameter of 10 μm, a diameter of 5 mm, and a thickness of 3 mm) was installed in the flow path between the injection valve 6 and the sample suction nozzle 8 of the apparatus.
Column 4: manufactured by Sekisui Chemical Co., Ltd., trade name “Micronex A1c HS-II” detector 5: manufactured by Shimadzu Corporation, SPD-6AV
Further, the filter F1 (a stainless sintered filter having a hole diameter of 5 μm, a diameter of 5 mm, and a thickness of 3 mm) shown in FIG. 4 was installed in the flow path between the injection valve 6 and the column 4.
[0020]
(Comparative Example 1)
A liquid chromatograph was assembled in the same manner as in Example 1 except that the filter F was not installed in the flow path between the injection valve 6 and the sample suction nozzle 8 of the automatic sample introduction device 3.
[0021]
Performance Evaluation The performance of the liquid chromatographs of Example 1 and Comparative Example 1 was evaluated as follows.
An eluent (100 mM phosphate buffer) was accommodated as the mobile phase 11 in the mobile phase container 1. In the sample container 9, 0.1 M phosphoric acid in which healthy human blood was dissolved as a sample [Triton X-100 (polyethylene glycol octyl phenyl ether, manufactured by Wako Pure Chemical Industries, Ltd.) dissolved at a concentration of 0.1 wt%. Buffer solution (pH 7)] was diluted 30 times with hemolysis. This mobile phase 11 is passed through the liquid feed pump 2 at a flow rate of 2 ml / min, and in this state, 500 μl of sample is injected into the column 4 every 3 minutes by the automatic sample introduction device 3, Analysis of hemoglobin A1c was performed. The filter F of Example 1 was automatically washed every 3 minutes. Regarding the pressure displayed by the liquid feeding pump during the analysis, the increase value was monitored, and the relationship with the number of sample injections was determined.
[0022]
[Table 1]

[0023]
In Table 1, the earlier the pressure rise, the shorter the life of the filter F1. Therefore, it can be seen from Table 1 that in the chromatograph of Example 1, the filter F can be effectively cleaned and the service life is extended, and the service life of the filter F1 is also extended.
[0024]
【The invention's effect】
The configuration of the liquid chromatograph of the present invention is as described above. Since a filter is installed in the flow path between the injection valve for sample injection and the sample suction nozzle, the direction in which the sample flows is opposite. By flowing the washing liquid, the filter can be washed and the clogging of the filter can be effectively removed, so that the life of the filter can be extended, and a liquid chromatograph that does not deteriorate the separation performance is provided. In addition, since an ordinary sample introduction device for liquid chromatography is equipped with a device for backwashing, the liquid chromatograph of the present invention can be produced by slightly improving the conventional liquid chromatograph device. it can.
[Brief description of the drawings]
FIG. 1 is a diagram showing a configuration of a liquid chromatograph of the present invention.
FIG. 2 is a diagram showing a connection state of an injection valve during sample inhalation.
FIG. 3 is a diagram showing a connection state of an injection valve when a sample is injected into a column.
FIG. 4 is a diagram showing a configuration of a conventional liquid chromatograph.
[Explanation of symbols]
DESCRIPTION OF SYMBOLS 1 Mobile phase container 2 Liquid feed pump 3 Sample introduction apparatus 4 Column 5 Detector 6 Injection valve 7 Aspirator 8 Sample suction nozzle 9 Sample container 11 Mobile phase F Filter F1, F2, F3 Filter a, b, c, d, e , F Connection port

Claims (1)

A filter is installed in the flow path between the injection valve for sample injection and the sample suction nozzle, and the injection valve, the sample suction nozzle and the filter have the same cleaning liquid and have a mechanism for cleaning during the measurement. A liquid chromatograph characterized by

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