WO2019043754A1

WO2019043754A1 - Flow vial

Info

Publication number: WO2019043754A1
Application number: PCT/JP2017/030722
Authority: WO
Inventors: 研壱保永
Original assignee: 株式会社島津製作所
Priority date: 2017-08-28
Filing date: 2017-08-28
Publication date: 2019-03-07
Also published as: JPWO2019043754A1; JP6753536B2

Abstract

This flow vial comprises: a vial body having a space that is open on the top and accommodates liquid therein, an inlet flow path that is in communication with a lower part of the space, and an outlet flow path that is in communication with an upper part of the space; a septum that is made up of an elastic material, has an outer diameter that is larger than the inner diameter of the opening of the vial body, is disposed directly above the opening, and seals the opening; and a cap that has a through hole for allowing a sampling needle to pass from the upper surface to the lower surface of the cap, has a recess on the lower surface thereof that has an inner diameter roughly the same as the outer diameter of the septum, is attached to the upper part of the vial body in a state where the septum has been fit into the recess, and pushes the septum into the edge of the opening of the vial body with the bottom surface of the recess.

Description

Flow vial

The present invention relates to a flow vial used in an analysis system for measuring a change over time of a sample, such as a dissolution rate of a dissolution test and a reaction rate of process synthesis.

In recent years, it has been proposed to use a liquid chromatograph in order to analyze the elution rate of the elution test and the reaction rate of the process synthesis over time, and it has been practiced (see Patent Document 1). In that case, a flow vial is installed as a sample container in a liquid chromatograph autosampler so that a sample to be analyzed can be introduced into the liquid chromatograph online.

Conventional flow vials have an inlet and an outlet on the upper and lower sides of a normal glass vial. The top opening of the flow vial is sealed by a septum made of an elastic material such as silicon. At sampling time, the sampling needle penetrates the septum, allowing the tip to penetrate into the flow vial and aspirates the sample in the flow vial from the tip.

Unexamined-Japanese-Patent No. 2006-118985

The septum that seals the upper surface of the flow vial elastically closes the through hole created by the penetration of the sampling needle after the sampling needle is withdrawn from the flow vial, and seals the upper surface of the flow vial again It is a thing. However, it has been found that when the pressure in the flow vial is increased, such as when replacing the liquid in the flow vial, the liquid may leak from the through hole formed by the penetration of the sampling needle. In particular, when the sampling needle penetrates the septum on the top surface of the flow vial a plurality of times, the through hole of the septum is widely spread, which further causes the liquid leakage.

Then, this invention aims at suppressing the liquid leak from the through-hole which arises in a septum by insertion and extraction of a sampling needle.

In the conventional glass flow vial, a septum is disposed to seal the opening on the upper surface of the vial body, and the cap attached so as to cover the top of the vial body presses the rim of the septum toward the vial body It has become. In this structure, since there is a gap between the outer circumferential surface of the septum and the inner surface of the cap, even if stress is applied to the septum by tightening the cap, the septum only deforms in the circumferential direction. That is, in the conventional flow vial structure, even if the cap is tightened tightly, no stress is generated in the direction to close the through hole of the septum resulting from the insertion and removal of the sampling needle.

The present invention improves the structure of the conventional flow vial as described above so that when the cap is tightened, stress is efficiently generated in the direction of closing the through hole of the septum produced by the insertion and removal of the sampling needle. , Control leakage from the septum.

That is, the flow vial according to the present invention has a space which is open at the top and contains a liquid therein, and has a vial body having an inlet flow passage communicating with the lower portion of the space and an outlet flow passage communicating with the upper portion of the space; A septum made of an elastic material having an outer diameter larger than the inner diameter of the opening of the vial body and disposed immediately above the opening to seal the opening, and for passing a sampling needle from the upper surface to the lower surface A recess having a through hole and an inner diameter substantially the same as the outer diameter of the septum is provided on the lower surface, and the septum is mounted on the top of the vial body in a state where the septum is fitted into the recess. A cap for pressing the septum against the edge of the opening of the vial body.

The depth dimension of the recess may be smaller than the thickness dimension of the septum.

In a preferred embodiment of the flow vial according to the present invention, a screw is provided on the outer peripheral surface of the lower portion of the cap, and the inner peripheral surface of the vial body is screwed with a screw on the outer peripheral surface of the lower portion of the cap. And the cap is configured such that a screw provided on the outer peripheral surface of the lower portion is attached by screwing with a screw on the non-recessed week surface of the vial body ing. That is, this embodiment is not mounted such that the top of the vial body is capped.

The flow vial is provided with an inlet channel at the lower side and an outlet channel at the upper side. However, if there is a space above the outlet channel, stagnation is likely to occur in that part, and the sample to be replaced There is a risk that air may remain above the outlet channel. In the structure in which the cap is mounted so that the upper part of the vial body is covered, it is difficult to provide the outlet flow path in the portion covered by the cap of the vial body. Therefore, a large space which becomes stagnant will be generated inside the part to which the cap is put.

On the other hand, in the above embodiment, since the lower portion of the cap is mounted so as to be fitted into the recess provided on the upper surface of the vial body, the outlet channel may be provided at a position close to the upper end of the internal space of the vial body Therefore, the space formed above the outlet channel can be reduced.

In the flow vial according to the present invention, the cap has a recess on the lower surface having an inner diameter substantially the same as the outer diameter of the septum, and the cap is attached to the top of the vial body with the septum fitted in the recess. Since the septum is configured to be pressed against the edge of the opening of the vial body at the bottom of the container, the septum whose outer peripheral surface is held by the recess of the cap is less likely to deform in the outer peripheral direction even when the cap is tightened. As a result, when the cap is tightened, stress is efficiently generated in the direction to close the through hole of the septum caused by the insertion and removal of the sampling needle, and the liquid leakage from the through hole caused in the septum by the insertion and removal of the sampling needle Be suppressed. In addition, since the inner diameter of the recess of the cap is substantially the same as the outer diameter of the septum, the septum is held by the cap, and the septum is simultaneously removed from the vial body when the cap is removed from the vial body. Septum replacement work is facilitated.

It is a schematic block diagram which shows an example of an analysis system. It is a schematic cross-section block diagram which shows an example of a structure in the auto sampler in which the flow vial was provided. It is a disassembled sectional view which shows the state of the flow vial before equipping a vial body with a cap. It is a disassembled sectional view which shows the state of a flow vial when a cap is attached to a vial body. It is an exploded sectional view showing the state of the flow vial when the cap is removed from the vial body.

Hereinafter, an embodiment of a flow vial according to the present invention will be described using the drawings.

First, an analysis system including an autosampler in which a flow vial to which the present invention is applied is used will be described with reference to FIG.

The analysis system includes a sample processing device 2, a liquid chromatograph 4, and an arithmetic processing device 6. Examples of the sample processing device 2 include a dissolution tester for performing a dissolution test of a drug or the like, a flow synthesis device for performing flow synthesis, and the like. The arithmetic processing unit 6 is, for example, a personal computer electrically connected to a system controller (not shown) for managing the

modules

8, 10, 12 and 14 of the liquid chromatograph 4.

The liquid chromatograph 4 includes a liquid delivery device 8, an auto sampler 10, a column oven 12, and a detector 14.

The liquid feeding device 8 is a device for feeding the mobile phase using a liquid feeding pump. The outlet of the liquid transfer device 8 is connected to the autosampler 10 through a pipe.

The autosampler 10 has a flow vial 26 (see FIG. 2) for containing a sample supplied from the sample processing apparatus 2 and a sampling needle 20 (see FIG. 2) for collecting a sample from the flow vial 26. And an injection port 22 (see FIG. 2) for injecting a sample collected by the sampling needle 20 into a flow path through which the mobile phase from the liquid transfer device 8 flows.

An analysis column (not shown) for separating the sample into components is housed in the column oven 12. The analytical column in the column oven 12 is connected to the outlet of the autosampler 10 via a pipe so that the sample injected by the autosampler 10 is introduced to the analytical column together with the mobile phase from the liquid transfer device 8 It is configured. The downstream end of the analysis column in the column oven 12 is connected to the detector 14 via piping.

The detector 14 is for detecting a sample component separated by the analysis column, and is, for example, an ultraviolet absorbance detector. The detector signal obtained by the detector 14 is taken into the arithmetic processing unit 6 and used for quantifying the concentration of the sample component.

As shown in FIG. 2, a sampling needle 20, an injection port 22, a collection container 24, and a flow vial 26 are provided in the autosampler 10. Although only one flow vial 26 is shown in the figure, a plurality of flow vials 26 are actually arranged in line in the direction perpendicular to the paper surface of the figure. The number of flow vials 26 is not limited.

The injection port 22 is for injecting the sample collected by the sampling needle 20 from the flow vial 26 into the analysis flow channel of the mobile phase. The injection port 22 is configured to insert the tip of the sampling needle 20 and connect the sampling needle 20 in a fluid-tight manner.

The collection container 24 is a container for temporarily storing the sample collected by the sampling needle 20 from the flow vial 26.

The flow vial 26 comprises a vial body 30, a cap 32 mounted on the top of the vial body 30, and a septum 34 made of an elastic material sandwiched between the vial body 30 and the cap 32. Inside the vial body 30, a space 30a for containing a sample, an inlet channel 36 communicating with the lower part of the space 30a, and an outlet channel 38 communicating with the upper part of the space 30a are provided. An inlet pipe 16 is connected to the inlet channel 36, and an outlet pipe 18 is connected to the outlet channel 38.

The space 30a inside the vial body 30 is open at the top, and the septum 34 is disposed immediately above the opening. The septum 34 is pressed by the cap 32 against the edge of the opening of the vial body 30.

The septum 34 is, for example, a disc-shaped silicon attached with a PTFE (polytetrafluoroethylene) sheet, but when the liquid supplied into the flow vial 30 is a strong solvent such as THF or chloroform A fluorine-based rubber may be used as the material of the septum 34 because silicon may melt.

The cap 32 is provided with a through hole 32b (see FIG. 3) communicating from the upper surface to the lower surface. The through hole 32 b of the cap 32 is for guiding the sampling needle 20 lowered from above to the space 30 a in the vial body 30. The sampling needle 20 lowered through the opening of the cap 32 penetrates the septum 34 and causes the tip to enter the space 30 a in the vial body 30 to aspirate the sample.

The sampling needle 20 is provided above the injection port 22, the collection container 24 and the flow vial rack 28. The sampling needle 20 is moved in the horizontal direction and in the vertical direction by the moving mechanism (not shown) with its tip directed vertically downward. The sampling needle 20 can aspirate the sample from the flow vial 26, discharge the sample into the collection container 24, and can aspirate the sample from the collection container 24 and inject the sample into the injection port 22. The sample injected through the injection port 22 is then introduced into the detector 14 through the analysis column in the column oven 12 by the mobile phase from the liquid delivery device 8.

The structure of the flow vial 26 will be described in more detail with reference to FIGS. 3 to 5.

The lower portion 32a of the cap 32 of the flow vial 26 has a cylindrical shape, and a screw is provided on its side surface. The upper surface of the vial body 30 is provided with a recess 30b having an inner diameter larger than the inner diameter of the inner space 30a leading to the inner space 30a. The inner diameter of the recess 30b is substantially the same as the outer diameter of the lower portion 32a of the cap 32, and a screw is provided on the inner peripheral surface of the recess 30b to be screwed with the screw on the outer peripheral surface of the lower portion 32a. That is, the cap 32 is mounted so as to be fitted into the recess 30 b on the upper surface of the vial body 30.

A recess 32 c of a shape into which the septum 34 is fitted is provided on the lower surface of the cap 32. In the case where the outer shape of the septum 34 has a disk shape, the recess 32 c is formed in a cylindrical shape. The recess 32 c is formed by a bottom surface and an annular protrusion formed in the outer peripheral portion of the bottom surface and having a predetermined thickness. The inner diameter of the recess 32 c is substantially the same as the outer diameter of the septum 34, and the depth dimension of the recess 32 c is smaller than the thickness dimension of the septum 34. Thus, when the septum 34 is attached to the recess 32c, the septum 34 slightly protrudes from the recess 32c. The thickness dimension of the septum 34 is, for example, about 3 mm, and the depth dimension of the recess 32 c is, for example, about 2 mm.

As shown in FIG. 4, the cap 32 with the septum 34 fitted in the recess 32 c is fitted in the recess 30 b of the vial body 30, and the cap 32 is rotated relative to the vial body 30. When it is tightened, only the lower surface of the septum 32 contacts the edge of the opening of the internal space 30a of the vial body 30. When the cap 32 is further tightened, the septum 32 is pressed toward the vial body 30 by the bottom surface of the recess 32 c. At this time, since the inner peripheral surface of the recess 32c of the cap 32 (that is, the inner peripheral surface of the annular projection forming the recess 32c) holds the outer peripheral surface of the septum 34, the septum 34 deforms in the outer peripheral direction There is nothing to do. Thus, the stress applied to the septum 34 by the tightening of the cap 32 acts toward the center of the septum 34. That is, the stress applied to the septum 34 by tightening the cap 32 acts in the direction to close the through hole formed in the septum 34 by the insertion and removal of the sampling needle 20, and the liquid leakage from the through hole formed in the septum 34 is suppressed.

Further, as shown in FIG. 4, when the cap 32 is tightened, the center of the lower surface of the septum 34 is deformed so as to be pushed into the internal space 30 a of the vial body 30. The end on the inner space 30 a side of the outlet flow passage 38 is provided at a position not blocked by a part of the septum 34 that has been pushed into the inner space 30 a.

When a part of the septum 34 is pushed into the inner space 30a, the liquid pool space present above the end on the inner space 30a side of the outlet flow passage 38 is advantageously reduced. The height of the outlet channel 38 is designed such that most of the space above the end on the inner space 30a side of the outlet channel 38 is filled with a part of the septum 34 that protrudes into the inner space 30a. It is done.

Also, as shown in FIG. 5, when the cap 32 is removed from the vial body 30, the septum 34 is also removed from the vial body 30 while being held on the lower surface of the cap 32. Therefore, the septum 34 does not remain in the recess 30 b on the upper surface of the vial body 30, and the operation such as replacement of the septum 34 can be easily performed.

DESCRIPTION OF SYMBOLS 2 sample processing apparatus 4 liquid chromatograph 6 arithmetic processing apparatus 8 liquid feeding apparatus 10 autosampler 12 column oven 14 detector 16 inlet piping 18 outlet piping 20 sampling needle 22 injection port 24 collection container 26 flow vial 28 flow vial rack 30 vial Body 30a Internal space 30b Recess 32 Cap 32a Cap lower part 32b Through hole 32c Indented 34 Septum 36 Inlet flow path 38 Exit flow path

Claims

A vial body having an opening at the top and containing a liquid therein, and an inlet channel communicating with a lower portion of the space and an outlet channel communicating with an upper portion of the space;
A septum made of an elastic material having an outer diameter larger than the inner diameter of the opening of the vial body and disposed immediately above the opening to seal the opening;
It has a through hole for penetrating a sampling needle from the upper surface to the lower surface and has a recess on the lower surface having an inner diameter substantially the same as the outer diameter of the septum, with the septum fitted in the recess A cap mounted on the top of the vial body and pressing the septum against the opening edge of the vial body at the bottom of the recess.
The flow vial according to claim 1, wherein the stress applied to the septum acts toward the center of the septum.
The flow vial according to claim 1, wherein a central lower surface of the septum protrudes into the space of the vial body through the opening.
The flow vial according to claim 1, wherein the depth dimension of the recess is smaller than the thickness dimension of the septum.
A screw is provided on the outer peripheral surface of the lower portion of the cap, and the vial body has on the upper surface a concave portion provided on the inner peripheral surface with a screw screwed with a screw on the outer peripheral surface of the lower portion of the cap 5. The cap according to any one of claims 1 to 4, wherein a screw provided on an outer peripheral surface of the lower portion is attached by screwing with a screw on an inner peripheral surface of the recess of the vial body. A flow vial as described in Item.