JPS5965245A - Apparatus for evaporative concentration or drying-up and re-dissolving of minute amount of specimen solution - Google Patents

Apparatus for evaporative concentration or drying-up and re-dissolving of minute amount of specimen solution

Info

Publication number
JPS5965245A
JPS5965245A JP57175161A JP17516182A JPS5965245A JP S5965245 A JPS5965245 A JP S5965245A JP 57175161 A JP57175161 A JP 57175161A JP 17516182 A JP17516182 A JP 17516182A JP S5965245 A JPS5965245 A JP S5965245A
Authority
JP
Japan
Prior art keywords
pipe
port
tube
tube member
solvent
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
Application number
JP57175161A
Other languages
Japanese (ja)
Inventor
Shoji Hara
昭二 原
Kitarou Oka
希太郎 岡
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Individual
Original Assignee
Individual
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Individual filed Critical Individual
Priority to JP57175161A priority Critical patent/JPS5965245A/en
Publication of JPS5965245A publication Critical patent/JPS5965245A/en
Pending legal-status Critical Current

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Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N25/00—Investigating or analyzing materials by the use of thermal means
    • G01N25/14—Investigating or analyzing materials by the use of thermal means by using distillation, extraction, sublimation, condensation, freezing, or crystallisation

Abstract

PURPOSE:To make it possible to treat a minute amount of a specimen in good efficiency, by a method wherein a rod member is inserted into a pipe withstanding vacuum and pressure so as to occupy almost the entire length of the pipe and an injection valve of a specimen liquid is provided to one end of the pipe while a valve having ports for exhausting gas and sending out a concentrate is provided to the other end thereof. CONSTITUTION:Into a fine pipe 1 withstanding vacuum and pressure such as a glass pipe, a rod member 2 made of a same material is inserted to reduce the space volume in the pipe while enlarge the evaporation area thereof. A valve 4 having a specimen solution injecting port (a) and a port (a') for injecting a solvent used in dissolving a dried-up specimen is mounted to one end of the pipe 1 while valve 5 having a port (bo) for evacuating or pressurizing the pipe 1, a port (b) communicated with a vacuum pump for holding reduce pressure and sucking the evaporated solvent and a port (b') for sending a liquid having a concentrate or a dried-up component re-dissolved therein to an analytical apparatus is mounted to the other end thereof and an apparatus 3 for heating the pipe 1 is mounted to form a conc. apparatus. A specimen liquid is supplied into the pipe one time-several times and, after concentrated under vacuum or evaporated to dryness, inert gas is sent into the pipe 1 from the port (bo) to bring the internal pressure of the pipe to atmospheric pressure while the solvent is put therein from the port (a') to send out the concentrate from the part (b') or the solvent is sent to the pipe 1 to send out the dried-up substance while redissolving it.

Description

【発明の詳細な説明】 〔ｌ〕発明の背景 本発明は、微少量の試料の溶液を蒸発濃縮ないし乾固お
よび再溶解するだめの装置に関する。DETAILED DESCRIPTION OF THE INVENTION [l] BACKGROUND OF THE INVENTION The present invention relates to an apparatus for evaporating, concentrating or drying and redissolving a minute amount of a sample solution.

試料の調製、合成、分析などの化学実験において、抽出
液などを蒸発に付して濃縮したのち、残渣ないし濃縮液
を再溶解して、次の工程に移行させるための送液からな
る一連の操作がひろ（用いられている。In chemical experiments such as sample preparation, synthesis, and analysis, it is a series of liquid transfer processes that involve evaporating and concentrating extracts, redissolving the residue or concentrated liquid, and moving on to the next process. Manipulation is Hiro (used.

この一連の操作では、各素工程が手動による不連続な操
作で行なわれているので、効率が良（ない。特に、水性
の生体試料の分析において、目的成分を抽出して粗分画
したのち、抽出液を蒸発濃縮ないし乾固してから再溶解
して、ガスクロマトグラフィーまたは液体りｐマドグラ
フィーに注入する操作では、これら各工程のスイッチン
グの連続化が要望されているところである。また、各素
工程を手動による不連続な操作で行なう場合には、試薬
類の蒸発にもとづく実験室内大気の汚染や試料の損失な
ども峨げ難い。In this series of operations, each elementary step is performed manually and discontinuously, so it is not efficient.Especially in the analysis of aqueous biological samples, the target components are extracted and roughly fractionated. In the operation of evaporating and concentrating the extract to dryness, redissolving it, and injecting it into gas chromatography or liquid plasma chromatography, continuous switching of each of these steps is desired.Also, When each elementary step is carried out manually and discontinuously, there is less risk of contamination of the laboratory atmosphere or loss of samples due to evaporation of reagents.

［１１〕発明の概要 要旨 本発明は上記の点に解決を与えることを目的とし、内部
に好ましくは進退自在に設けた棒体を有を達成しようと
するものである。[11] Summary of the Invention The present invention aims to provide a solution to the above-mentioned problems, and is intended to provide a rod body preferably provided inside the rod body so as to be movable forward and backward.

従って、本発明による微少量試料溶液の蒸発濃縮ないし
乾１１′１および再溶解のだめの装置は、減圧および加
圧に耐える管部拐と、その内部に収容されて該管内部の
実質的に全長にわたって存在するＩＮ部材と、該ゞ１：
′ｆ部材の一端に設けられた、該管内部を試料溶液源お
よび溶媒源と連通させるための弁機４７ηと、該背部材
の他殉に設けられた、該管部材内部を再溶７１ＪＴｌｌ
ｆ＋液受容装置および減圧発生源と連通させるだめの弁
（幾構とからなり、該管部材の内径が３　ｎ１ｌＲ以下
であって微少ｉの試料溶液の蒸発濃縮ないし乾ｌｉｄお
よび再溶解が可能なものであること、全特徴とするもの
である。Therefore, the device for evaporating concentration or drying 11'1 and redissolving a small amount of sample solution according to the present invention includes a tube section that can withstand reduced pressure and increased pressure, and a tube section that is accommodated within the tube section and that extends substantially over the entire length of the tube section. IN members that exist over 1:
'f A valve 47η provided at one end of the member for communicating the inside of the tube with a sample solution source and a solvent source, and a valve 47η provided in addition to the back member for remelting the inside of the tube member 71JTll
A reservoir valve (consisting of several pieces) that communicates with the f+ liquid receiving device and the reduced pressure generation source, the inner diameter of the tube member being 3 n1lR or less, and capable of evaporating concentration or drying and redissolving a minute sample solution It is something that is a thing, a thing that has all its characteristics.

また、本発明によるもう一つの微少量試料溶液の蒸発濃
縮ないし乾固および再溶解のための装置は、減圧および
加圧に耐える管部材と、その内部に外部から進退自在に
収容されて核管部材内部の実質的に全長にわたって存在
しうる棒部材と、該管部材の一端に設けられた。該棒部
材を該管部材内部に外部から進退自在に保持するだめの
棒保持機構と、積管部材の一端に設けられた、該管部材
内部を試料溶液源および溶媒源と連通させるための弁機
構と、該管部材の他端に設けられた、該管部材内部を再
溶解溶液受容装置ａおよび減圧ないし加圧発生源と連通
させるだめの弁機構とからなり、該管部材の内径が１５
　ｔｙｍ以下であって微少量の試料溶液の蒸発濃縮ない
し乾固および再溶解が可能なものであること、全特徴と
するものである。Another apparatus according to the present invention for evaporating, concentrating, drying, and redissolving a minute sample solution includes a tube member that can withstand reduced pressure and pressurization, and a nuclear tube housed inside the tube member so as to be able to move forward and backward from the outside. A rod member may be present for substantially the entire length inside the member, and a rod member may be provided at one end of the tube member. a retainer rod holding mechanism that holds the rod member inside the tube member so that it can move forward and backward from the outside; and a valve provided at one end of the stacked tube member for communicating the inside of the tube member with a sample solution source and a solvent source. and a valve mechanism provided at the other end of the tube member for communicating the inside of the tube member with the redissolved solution receiving device a and the reduced pressure or pressurization source, and the inner diameter of the tube member is 15 mm.
tym or less and that it is possible to evaporate, concentrate, dry, and redissolve a very small amount of sample solution.

効果 本発明装置４によれば、微少量の試料をその損失が少な
（しかも前記の諸問題を伴なうことなく処理することが
できる。特に、本発明装置によって再溶解されて調製さ
れた試料溶液は他の装置に直接スイッチすることかでき
るので、本発明装置ケインターフェースとして、たとえ
ば逆相および順相のようにモードの異なる二つの液体ク
ロマトグラフィーカラムのスイッチングを行なうことが
できる。具体的には、たとえば、水浴液の試料から目的
物を抽出ないし分画したのち、新らたな溶媒に溶解させ
た試料溶液全調製し、オンラインで第二の分析カラムに
注入するという操作が可能である。Effects According to the device 4 of the present invention, it is possible to process a very small amount of sample with little loss (and without the above-mentioned problems. In particular, it is possible to process a sample that has been redissolved and prepared by the device of the present invention). Since the solution can be directly switched to another device, the device interface of the present invention can be used to switch between two liquid chromatography columns with different modes, such as reverse phase and normal phase. For example, it is possible to extract or fractionate the target substance from a sample of water bath liquid, then dissolve the sample solution in a new solvent, prepare the entire sample solution, and inject it online into the second analytical column. .

また、本発明装置に使用されている管部材は、これを取
外し自在に構成することができ、そのようにｔｆ！７成
した場合は管内面に試料を析出付着させたまへ管端を閉
止して、試料の保存、輸送等を有利に行なうことができ
る。Further, the tube member used in the device of the present invention can be configured to be removable, so that the tf! 7. When the sample is deposited and adhered to the inner surface of the tube, the end of the tube is immediately closed, and the sample can be stored, transported, etc. advantageously.

１）　　イｊり　　　成 第１図は、本発明装置の一具体例全模式的に示す説明図
である。1) Illustration FIG. 1 is an explanatory diagram schematically showing a specific example of the apparatus of the present invention.

この具体例は、管部材の内部に棒部材が封入されていて
進退しない形式のものであり、機能的にいえば再溶解溶
媒量の調節を行なわない型式のものである。この型式は
、再溶解溶媒量が一定の場合に、特に溶媒量が少ないと
きに有効である。This specific example is of a type in which a rod member is enclosed inside a tube member and does not move forward or backward, and functionally speaking, it is a type in which the amount of redissolved solvent is not adjusted. This type is effective when the amount of redissolved solvent is constant, especially when the amount of solvent is small.

第１図において、管部材１は、所要長さ全確保するため
蛇管状に配設されているが、直線状またはコイル状その
仙台目的的な任意の形状をとり５ることはいうまでもな
い。管部材１は、ポリテトラフルオロエチレン（ＰＴＦ
Ｅ　）　、ガラス、ステンレス鋼、その他の耐薬品性の
材料により、所定の加圧ないし減圧に耐えるような肉厚
をもって製作される。管部材ｌの一例金挙げれば、内径
０．５〜２　ｍｍ程度で長さｌＱ　ｔ＊　〜ｌ　ｍ程度
のＰＴＦＥ製の丸管がある。管部材の内面には、小溝ま
たは小凹陥部を刻設してもよい。In FIG. 1, the pipe member 1 is arranged in a serpentine shape to ensure the entire required length, but it goes without saying that it may take any desired shape such as a straight line or a coil. . The pipe member 1 is made of polytetrafluoroethylene (PTF
E) Manufactured from glass, stainless steel, or other chemical-resistant material with a wall thickness that can withstand the specified pressure or vacuum. An example of the tube member l is a round tube made of PTFE with an inner diameter of about 0.5 to 2 mm and a length of about lQt* to lm. A small groove or a small recess may be carved on the inner surface of the tube member.

棒部材２も、上記のような材料で製作される。The rod member 2 is also made of the materials mentioned above.

その長さは管部拐１の実質的全長にわたって存在しうる
程度でありまたその直径は管部材１の内径とあまり差が
ないこと、すなわち管内の自由空間があまり太き（ない
こと、が好ましい。−例１［げれば、直径０．２〜１．
５朋程度のステンレス鋼またはＰＴＦＥの丸棒がある。It is preferable that its length is such that it can exist over substantially the entire length of the tube member 1, and its diameter is not much different from the inner diameter of the tube member 1, that is, the free space inside the tube is not too thick. - Example 1 [If the diameter is 0.2 to 1.
There is a stainless steel or PTFE round bar of about 5 mm.

管部材１は、温度調節装置３内に収容されていて、管部
材内部の温度を所定値に保てるようにしである。温度調
節装置の一例を挙げれば、冷〜温水槽がある。電熱によ
る方式が可能なことはいう管部拐１には、その入口部お
よび出口端にそれぞれ弁機構４および５が接続されてい
る。The tube member 1 is housed in a temperature control device 3, so that the temperature inside the tube member can be maintained at a predetermined value. An example of a temperature control device is a cold to hot water tank. The tube section 1, which can be operated by electric heating, has valve mechanisms 4 and 5 connected to its inlet and outlet ends, respectively.

大口弁ｉｎｌ　ｆｔ’ｊ　４は、管部材１の内部を試料
溶液源および溶媒臨（いずれも図示されていない）と連
通させるだめのものであるが、必要に応じて管部材内部
全減圧ないし加圧発生源と連通させる機能を持っていて
もよい。The large mouth valve inl ft'j 4 is for communicating the inside of the tube member 1 with a sample solution source and a solvent supply (none of which are shown), but it can be used to completely reduce or increase the pressure inside the tube member as necessary. It may have a function of communicating with a pressure generating source.

出口弁Ｕ５ｋ　４’：・￥５は、管部材１の内部を再溶
解溶液受答装置δおよび減圧ないし加圧発生源（いずれ
も図示されていない）と連通させるだめのものである。The outlet valve U5k4':.¥5 is for communicating the inside of the pipe member 1 with the redissolved solution receiving device δ and a reduced pressure or pressurized source (none of which is shown).

ここで「加圧」とは管部材内部が常圧より高い圧力にあ
るということの外に、減圧状態による管部材内部がそれ
より高い圧力たとえば常圧に戻ることをも意味するもの
とする。その場合の加圧用のガスは、窒素、アルゴンそ
の他の不活性ガスであることが望ましい。Here, "pressurization" means not only that the inside of the tube member is at a pressure higher than normal pressure, but also that the inside of the tube member returns to a higher pressure, such as normal pressure, due to a reduced pressure state. In this case, the pressurizing gas is preferably nitrogen, argon, or other inert gas.

本発明で「再溶解溶液受容装置」という場合は、単純な
貯槽の外に、試料溶液を受入れてこれを分析する装置（
たとえばクロマトグラフ装置）をも意味するものである
。再溶解溶液受容装置が本発明装置に直結した分析装置
でありうることが本発明の利点であることは前記したと
ころである。In the present invention, the term "redissolved solution receiving device" refers to a device that receives a sample solution and analyzes it (in addition to a simple storage tank).
For example, it also means a chromatographic device). As mentioned above, it is an advantage of the present invention that the redissolved solution receiving device can be an analysis device directly connected to the device of the present invention.

２）操作 この装置は、下記の通りに操作される。すなわち、試料
の有機溶媒溶液は、送液ポンプ（図示されていない）に
より入口弁ｉ構４のポートａより管部材１内に導入され
る。管部材１は温水ジャケット３により所定温度に加温
されており、またその内部は出口弁機構５のポー）ｂに
接続された減圧ポンプ（図示されていない）によって減
圧にされる。管部材１内部の温度および減圧の程度は、
使用した有機溶媒の沸点に応じて調節して、管部材１の
内面および棒部材２の表面で円滑な蒸発がおこるように
する。蒸発した溶媒は、出口弁機構５のボートｂより排
出される。−回にある℃・昏マ複数回に分けて試料溶液
ｋｎ人して所定量の試料が管部材１内に１７３＞縮ない
し析出したところで、入口弁機構４を閉にし、出口弁機
構５を作動させてポー）ｂ。より窒素ガス′（ｉｌ−導
入して、管部材１の内部を常圧前後とする。そこで、弁
機構４のボートａ′　より再溶解のだめの溶媒を送ると
、管部材１の内面および棒部材２の表面の析出試料は再
溶解されて、弁機構５に至る。弁機構５を作動させて、
ポートｂ′　　より再溶解溶液をその受容装置（図示さ
れていない）、たとえばクロマトグラフ装置へと送る。2) Operation This device is operated as follows. That is, the organic solvent solution of the sample is introduced into the pipe member 1 from the port a of the inlet valve i structure 4 by a liquid pump (not shown). The pipe member 1 is heated to a predetermined temperature by a hot water jacket 3, and its interior is reduced in pressure by a pressure reducing pump (not shown) connected to a port (b) of an outlet valve mechanism 5. The temperature and degree of pressure reduction inside the pipe member 1 are as follows:
The boiling point of the organic solvent used is adjusted so that smooth evaporation occurs on the inner surface of the tube member 1 and the surface of the rod member 2. The evaporated solvent is discharged from the boat b of the outlet valve mechanism 5. When a predetermined amount of the sample has shrunk or precipitated in the tube member 1, the inlet valve mechanism 4 is closed and the outlet valve mechanism 5 is closed. Activate it and turn it on) b. Nitrogen gas' (il-) is introduced to bring the inside of the tube member 1 to around normal pressure. Then, when the solvent for redissolution is sent from the boat a' of the valve mechanism 4, the inner surface of the tube member 1 and the rod member The precipitated sample on the surface of 2 is redissolved and reaches the valve mechanism 5. The valve mechanism 5 is operated,
Port b' sends the reconstitution solution to its receiving device (not shown), such as a chromatographic device.

２、装（１りの他の具体例 １）構成 第２図は、本発明装置の他の具体例を模式的に示す説明
図である。2. Configuration of the device (one other specific example 1) FIG. 2 is an explanatory diagram schematically showing another specific example of the device of the present invention.

この具体例は、棒部材が管部材内部に外部から進退自在
に収容されて管部材内部の実質的に全長にわたって存在
しうるように４？＃成された型式のものであり、機能的
にいえば再溶解溶媒址の調節を行なうことのできる型式
のものである。この型式は、試料浴液の量が多い場合に
適しており、再溶解溶媒−はを自由に調節できるという
利点を有する。In this specific example, the rod member is housed inside the tube member so as to be freely advanced and retracted from the outside, and can be present over substantially the entire length inside the tube member. Functionally speaking, it is a type that can control the amount of redissolution solvent. This type is suitable when the amount of sample bath liquid is large, and has the advantage that the redissolution solvent can be freely adjusted.

なお、下記の説明において特に言及されていない事項は
、矛１１１シない限り前記の具体例について述べたとこ
ろがあてはまる。Note that for matters not specifically mentioned in the following description, the same as described with respect to the above-mentioned specific example applies unless otherwise specified.

第２図において、管部材１１は曲がり維（製作されてい
て、内径１５　＋ｒｒｍ以下、好ましくはｌＱＩＩ１ｍ
以下、具体的には内径４〜ＩＱ　１１１１１程度、長さ
５〜３０工程度の耐圧ガラス製またはステンレス６ｉ１
．１］製の丸管がある。In FIG. 2, the tubular member 11 is made of bent fibers with an inner diameter of 15 + rrm or less, preferably lQII1 m
Below, specifically, it is made of pressure-resistant glass or stainless steel 6I1 with an inner diameter of about 4 to IQ 11111 and a length of 5 to 30 steps.
．． There is a round tube made by 1].

棒部材１２も曲がり離（製作されていて、直径が上記管
部制の内径よりも０．５〜ｌ　ＩＲｍ程小さいもの、具
体的には直径３．５〜１４市程度のガラスまたはステン
レス鋼の丸棒である。棒部材の直径は管部材の内径より
僅かに小さく　ｌＰめて、管部材内部の自由空間がなる
べ（小さくなるようにするのが望ましい。また、その長
さは棒部材を管部材内に最大限に進入させてなおかつ管
部材入口においてそれを把持しうる程度のものと丁べき
である。The rod member 12 is also bent apart (made of glass or stainless steel with a diameter of 0.5 to 1 IRm smaller than the inner diameter of the tube control, specifically, a diameter of about 3.5 to 14 cm). It is a round rod.The diameter of the rod member is slightly smaller than the inner diameter of the tube member, so that the free space inside the tube member is preferably as small as possible.Also, the length of the rod member is It should be of such a size that it can be inserted into the pipe member as far as possible and still be able to grasp it at the entrance of the pipe member.

管部材の外部には温度調節装置１３が設けであること、
および管部材の入口および出口に弁機構１４および１５
が設けであること、ならびにこれらの機能は、前記第１
図の具体例の場合と全く同じである。A temperature control device 13 is provided on the outside of the pipe member;
and valve mechanisms 14 and 15 at the inlet and outlet of the tubular member.
are provided, and these functions are the same as those described in the first
This is exactly the same as the specific example shown in the figure.

枠部材１２を管部材１１の内部に進入させかつそこから
退出させるだめの保持機４’ｉ”Ｉ：は、ピストン棒の
保持に慣用されるような合目的的な任意のものでありう
る。図示の例では、棒部材１２の延長部１２′全ガイド
磯＄：’７１６によって、棒部材１２の進退時に管部材
内部に接触しないように保持している。棒部材１２は、
回転させて進退させることも可能である。The retainer 4'i''I: which allows the frame member 12 to enter and exit the interior of the tube member 11 can be of any suitable type, such as is customary for retaining piston rods. In the illustrated example, the extension portion 12' of the rod member 12 is held so as not to come into contact with the inside of the tube member when the rod member 12 moves back and forth.
It is also possible to move it forward and backward by rotating it.

２）操作 梓部月１２ヲ最大限に引出して管部材１１の内部全学に
しておいて、大ロ弁機構１４ヲ作動させて試料溶液金管
部材内部に心入する。出口弁機構１５のボー）ｂより管
部材内部を吸引して減圧にすると共に温度調節装置１３
により加熱を行なって、管部材内の試料溶液から溶媒全
蒸発さぜる。蒸発残渣は、管部材１１の内面の導入口に
近い場所に濃縮ないし析出するようにする。すなわち、
サンプルの飛沫がとんで損失がおこるため入口にとどめ
ることが好ましい。2) Operation Pull out the opening 12 to the maximum extent to cover the entire inside of the tube member 11, and operate the large valve mechanism 14 to insert the sample solution into the inside of the tube member. The inside of the pipe member is suctioned from the bow of the outlet valve mechanism 15 to reduce the pressure, and the temperature control device 13
Heating is performed to completely evaporate the solvent from the sample solution in the tube member. The evaporation residue is concentrated or deposited on the inner surface of the tube member 11 near the inlet. That is,
It is preferable to keep the sample at the entrance because the droplets of the sample fly off and cause loss.

所定量の試料ないし蒸発残渣が生成したところで、棒部
材１２ヲ適当深さまで進入させ、出口弁機構１５を作動
させてポートｂ。より窒素ガスヲ樽入して管部材内部を
常圧前後としたのち、入口弁機’＋４’４１４　ｋ作動
させてポートａ′　　より再溶解溶媒全導入する。管ｔ
５１１材１１内面に付着している試料残渣は、枠部材１
２との間の狭い空間に侵入してくる再溶解溶媒に溶解さ
れ、生成溶液は出１０弁機構１５のポートｂ′　　より
排出されて、再溶解浴液受容装置（図示されていない）
に送られる。When a predetermined amount of sample or evaporation residue is generated, the rod member 12 is advanced to an appropriate depth, the outlet valve mechanism 15 is operated, and the port b is removed. After introducing a nitrogen gas barrel to bring the inside of the pipe member to around normal pressure, the inlet valve '+4'414k is operated to introduce all of the redissolving solvent from port a'. tube t
The sample residue adhering to the inner surface of the 511 material 11 is removed from the frame member 1.
The produced solution is dissolved in the redissolution solvent that enters the narrow space between the two and the resulting solution is discharged from the port b' of the output valve mechanism 15 and transferred to the redissolution bath liquid receiving device (not shown).
sent to.

管部旧１１内の自由空間は枠部利１２の進入程度によっ
て調節することができ、それによって試料量および再溶
解溶媒量をある範囲内で自由に調節することができる。The free space within the tube part 11 can be adjusted by the degree of intrusion of the frame part 12, thereby making it possible to freely adjust the amount of sample and the amount of redissolving solvent within a certain range.

第３図は、本発明装置ｌｌ　ｋ分析装置内に組み込んで
具体的に利用する場合を示す説明図である。FIG. 3 is an explanatory diagram showing a case in which the device of the present invention is incorporated into an analyzer and used specifically.

１）分析装置系 紀３図において、鎖線で囲んだ区域すが不発明装置（お
よび付帯装置）による蒸発−再溶解一注人工程に係る。1) Analyzer System In Figure 3, the area surrounded by chain lines relates to the evaporation-remelting process using the uninvented equipment (and ancillary equipment).

区域ａは抽出工程ないし試料作製工程、区域Ｃは最終的
な分離分析のためのクロマトグラフ分析工程である。Zone a is an extraction step or sample preparation step, and zone C is a chromatographic analysis step for final separation analysis.

区域ａは、抽出溶媒としてのジエチルエーテルの予備的
精製、水飽和のための液滴をつ（る装置（管１０１　、
１０２　、１０３　）と、試料の注入口１０４、篩効率
ケイソウ上充填カラム１０５、およびＵＶモニター１１
０からなりたつ。Area a includes droplet collection equipment (tube 101,
102 , 103 ), a sample inlet 104 , a sieve efficiency diatomaceous packed column 105 , and a UV monitor 11
Consists of 0.

区域すでは、前記第一の具体例（第１図）（たｙし、青
部月はＵ字型に構成しである）による本発明装置１０７
（管部材は内径１　ｎｕｎのステンレス丸管、枠部（・
４は直径０．９＋ｎｍ、長さ４５−のステンレス丸棒）
を減圧発生源であるアスピレータＡに連結して管部材内
を減圧にし、抽出カラムからスイッチされたジエチルエ
ーテル溶液を蒸発させる。蒸発残ｌｔｔは、弁装置１０
８の切換によって区域Ｃの液体クロマトグラフ装置の送
液系１０Ｇから導かれた浴離液に溶解されて、分析カラ
ム１０９に注入される。In the area, the device 107 of the present invention according to the first specific example (FIG. 1) (the Aobe moon is configured in a U-shape)
(The tube member is a stainless steel round tube with an inner diameter of 1 mm, and the frame part (
4 is a stainless steel round bar with a diameter of 0.9+nm and a length of 45-)
is connected to aspirator A, which is a source of reduced pressure, to create a reduced pressure in the tube member and evaporate the diethyl ether solution switched from the extraction column. The evaporation residue ltt is removed by the valve device 10.
8, the liquid is dissolved in the bath separation liquid led from the liquid delivery system 10G of the liquid chromatograph apparatus in zone C, and is injected into the analytical column 109.

これら工区域は、ＰＴＦＥ管で連結されており、また各
区域の’（（１，源をシーケンサにつないで自動化する
ことができる。These work areas are connected by PTFE pipes, and the '(1) source of each area can be connected to a sequencer for automation.

２）分析実験 上記の分析装置系音用いて、カフェイン’Ｔｈ　＃ｌｊ
用や しだ人尿中のカフェイン未変化体の定量について述べる
。従来はパッチ法により分析され、連続操作による方法
は知られていない。そこで水分析装置？適用してフロー
による連続分析を行なった。2) Analytical experiment Using the above analyzer system sound, caffeine 'Th #lj
This paper describes the determination of unchanged caffeine in human urine. Conventionally, analysis has been performed using a patch method, and no method using continuous operation is known. A water analyzer there? Continuous flow analysis was performed by applying this method.

高効率ケイソウ土充填カラム１０５として内径４ｍｍ、
長さ１０６Ｌ、分析カラム１０９として内径４１ｆｆｍ
。As a high efficiency diatomaceous earth packed column 105, the inner diameter is 4 mm,
Length 106L, inner diameter 41ffm as analysis column 109
.

長さ２０ｃｍの高効率シリカゲルカラム全使用する。A high-efficiency silica gel column with a length of 20 cm is used in its entirety.

定量の基硅データとして検量線を作製した。カフェイン
７５．１５０および３００ｎｇ金加えた正常人の尿１０
μｌｉ注入口１０４に注入する。水を飽和したジエチル
エーテルｋ１ｍｌ／ｍｉｎで送液する。試料注入後８分
間の抽出溶媒を本発明の蒸発管に導きながら、蒸発管の
他端から約２０１１１１１１　Ｆ（ｇの減圧で吸引し、
蒸発管内壁で抽出液を蒸発させる。この時蒸発管の外部
に約５０℃の温水全通過させる。加温により蒸発管内壁
に残る水滴（含水抽出液中の水に由来する）は蒸発消失
し、蒸発管内壁に抽出残渣が残留する。引続いて分析用
の溶離液として、ｎ−・ヘキサン／エタノール／メタノ
ール（４３：５０ニア　％　ｖ／ｖ　）　ｆ流速０　、
：３６＋ｙ＋Ｉ／ｍｉｎで蒸発管に送液する。溶離液は
蒸発管内に残留する抽出物全溶解しつつ分析カラムに注
入される。A calibration curve was prepared as basic data for quantitative determination. Normal human urine with caffeine 75.150 and 300 ng gold 10
Inject into μli injection port 104. Water is pumped with saturated diethyl ether at a rate of 1 ml/min. While introducing the extraction solvent for 8 minutes after sample injection into the evaporation tube of the present invention, about 20111111 F (g) was suctioned from the other end of the evaporation tube at a reduced pressure.
The extract is evaporated on the inner wall of the evaporation tube. At this time, all of the hot water at about 50°C is passed through the outside of the evaporation tube. By heating, water droplets (derived from water in the aqueous extract) remaining on the inner wall of the evaporation tube evaporate and disappear, leaving an extraction residue on the inner wall of the evaporation tube. Subsequently, n-hexane/ethanol/methanol (43:50 % v/v) was used as the eluent for analysis, with a flow rate of 0;
: Send the liquid to the evaporation tube at 36+y+I/min. The eluent is injected into the analytical column while completely dissolving the extract remaining in the evaporation tube.

カラムから浴出したカフェイン’ｃ　２４０　ｎｍ　（
Ｄ紫外腺で検出し、そのピーク高さから作製した検量線
（第４図）は原点を通る直線を与えた。また別に同情の
カフェインを抽出カラム１０５ヲ通過させることなく、
直接分析カラム１０９に注入した場合、それぞれ同一の
ピーク高さを与えることから、尿中のカフェインは損失
が無く、定量的に抽出、蒸発、移送されることが確認さ
れた。Caffeine 'c 240 nm (
The calibration curve (Fig. 4) prepared from the peak height detected by the D ultraviolet gland gave a straight line passing through the origin. Also, without passing the sympathetic caffeine through the extraction column 105,
When directly injected into the analysis column 109, the same peak height was obtained, confirming that caffeine in urine was quantitatively extracted, evaporated, and transferred without loss.

そこでカフエイフ１４０ｍｇ’ｅ経口投与した成人の原
音２時間後から毎２時間おきに採取した試料について未
変化体の定に４に行なった。投与後８時間後までの総排
出量を測定すると約３ｍｇであった。この装置は尿中の
目的成分の連続定量システムとして適切に作動すること
が確められた。Therefore, samples taken every 2 hours from 2 hours after the original sound to adults who had been orally administered 140 mg'e of Caffeif were subjected to 4 tests to determine the unchanged drug. The total excretion amount measured up to 8 hours after administration was approximately 3 mg. It was confirmed that this device works properly as a system for continuous determination of target components in urine.

【図面の簡単な説明】[Brief explanation of drawings]

第１〜２図は、本発明装置の具体例？示す説明図である
。 第３図は、本発明装置を組込んだ分析装置系を示す説明
図である。 第４図は、本発明装置を使用して尿中のカフェインを分
析する場合のカフェインの検量線を示すグラフである。 出願人代理人　　　猪　股　　　　清 ＝２（ ５３　図 −２６４− 邪　４　口Are Figures 1 and 2 a specific example of the device of the present invention? FIG. FIG. 3 is an explanatory diagram showing an analyzer system incorporating the device of the present invention. FIG. 4 is a graph showing a calibration curve for caffeine when analyzing caffeine in urine using the apparatus of the present invention. Applicant's agent Kiyoshi Inomata = 2 (53 Figure-264- Evil 4 Mouth

Claims (1)

【特許請求の範囲】 １、減圧および加圧に耐える管部材と、その内部に収容
されて該管部材内部の実質的に全長にわたって存在する
棒部材と、該管部材の一端に設けられた、該管部材内部
を試料溶液源および溶媒源叶戯Ｈｈ腎曖源と連通させる
だめの弁機構と、該管部材の他端に設けられた、該管部
材内部を再溶解溶液受容装置および減圧ないし加圧発生
源と連通させるための弁機構とからなり、該管部材の内
径が３朋以下であって微少量の試料溶液の蒸発濃縮ない
し乾固および再溶解が可能なものであること全特徴とす
る、微少量試料溶液の蒸発濃縮ないし乾固および再溶解
のだめの装置。 ２、減圧および加圧に耐える管部材と、その内部に外部
から進退自在に収容されて該管部材内部の実質的に全長
にわたって存在しうる棒部材と、該管部材の一端に設け
られた、該棒部材を該管部材内部に外部から進退自在に
保持するだめの棒保持機構と、該管部材の一端に設けら
れた、該管部材内部を試料溶液源および溶媒源と連通さ
せるだめの弁機構と、該管部材の他端に設けられた、該
管部材内部を再溶解溶液受容装置および減圧ないし加圧
発生源と連通させるだめの弁機構とからなり、該管部材
の内径が１５　ｍｍ以下であって微少量の試料溶液の蒸
発濃縮ないし乾固および再溶解が可能なものであること
を特徴とする、微少量試料溶液の蒸発濃縮ないし乾固お
よび再溶解のだめの装置。[Claims] 1. A pipe member that can withstand reduced pressure and pressurization, a rod member housed inside the pipe member and existing over substantially the entire length inside the pipe member, and provided at one end of the pipe member. A valve mechanism for communicating the inside of the tube member with a sample solution source and a solvent source, and a redissolution solution receiving device and a vacuum or It consists of a valve mechanism for communicating with a pressurized source, the inner diameter of the tube member is 3 mm or less, and it is capable of evaporating, concentrating, drying, and redissolving a minute amount of sample solution.All characteristics. A device for evaporating, concentrating, drying, and redissolving minute amounts of sample solutions. 2. A pipe member that can withstand reduced pressure and pressurization; a rod member that is housed inside the pipe member so as to be freely advanced and retractable from the outside and can exist over substantially the entire length inside the pipe member; and a rod member provided at one end of the pipe member; a retainer rod holding mechanism that holds the rod member inside the tube member so as to be freely advanced and retractable from the outside; and a retainer valve provided at one end of the tube member that communicates the inside of the tube member with a sample solution source and a solvent source. and a valve mechanism provided at the other end of the tube member for communicating the interior of the tube member with a redissolution solution receiving device and a reduced pressure or pressurization source, and the inner diameter of the tube member is 15 mm. 1. An apparatus for evaporating and concentrating or drying and redissolving a minute amount of a sample solution, which is capable of evaporating and concentrating or drying and redissolving a minute amount of the sample solution.
JP57175161A 1982-10-05 1982-10-05 Apparatus for evaporative concentration or drying-up and re-dissolving of minute amount of specimen solution Pending JPS5965245A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP57175161A JPS5965245A (en) 1982-10-05 1982-10-05 Apparatus for evaporative concentration or drying-up and re-dissolving of minute amount of specimen solution

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP57175161A JPS5965245A (en) 1982-10-05 1982-10-05 Apparatus for evaporative concentration or drying-up and re-dissolving of minute amount of specimen solution

Publications (1)

Publication Number Publication Date
JPS5965245A true JPS5965245A (en) 1984-04-13

Family

ID=15991324

Family Applications (1)

Application Number Title Priority Date Filing Date
JP57175161A Pending JPS5965245A (en) 1982-10-05 1982-10-05 Apparatus for evaporative concentration or drying-up and re-dissolving of minute amount of specimen solution

Country Status (1)

Country Link
JP (1) JPS5965245A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7790007B2 (en) 2005-11-29 2010-09-07 Nec Corporation Electrophoresis chip, electrophoresis apparatus, and method for analyzing a sample
JP2014182037A (en) * 2013-03-19 2014-09-29 Toyota Central R&D Labs Inc Volatile cracked component collection and recovery device, liquid chromatograph and volatile cracked component analysis method

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7790007B2 (en) 2005-11-29 2010-09-07 Nec Corporation Electrophoresis chip, electrophoresis apparatus, and method for analyzing a sample
JP2014182037A (en) * 2013-03-19 2014-09-29 Toyota Central R&D Labs Inc Volatile cracked component collection and recovery device, liquid chromatograph and volatile cracked component analysis method

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