JPH04194751A - Measuring method of concentration of trichloroacetic acid - Google Patents
Measuring method of concentration of trichloroacetic acidInfo
- Publication number
- JPH04194751A JPH04194751A JP32712990A JP32712990A JPH04194751A JP H04194751 A JPH04194751 A JP H04194751A JP 32712990 A JP32712990 A JP 32712990A JP 32712990 A JP32712990 A JP 32712990A JP H04194751 A JPH04194751 A JP H04194751A
- Authority
- JP
- Japan
- Prior art keywords
- trichloroacetic acid
- concentration
- chloroform
- measurement
- sample
- 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
Links
- YNJBWRMUSHSURL-UHFFFAOYSA-N trichloroacetic acid Chemical compound OC(=O)C(Cl)(Cl)Cl YNJBWRMUSHSURL-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 17
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims abstract description 38
- 238000005259 measurement Methods 0.000 claims abstract description 24
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- 239000000126 substance Substances 0.000 claims abstract description 12
- 238000004817 gas chromatography Methods 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 abstract description 9
- 230000035945 sensitivity Effects 0.000 abstract description 6
- 150000004702 methyl esters Chemical class 0.000 abstract description 4
- 238000005979 thermal decomposition reaction Methods 0.000 abstract description 3
- 239000012808 vapor phase Substances 0.000 abstract 2
- 235000011089 carbon dioxide Nutrition 0.000 abstract 1
- 239000000463 material Substances 0.000 abstract 1
- 210000002700 urine Anatomy 0.000 description 16
- 239000007789 gas Substances 0.000 description 14
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 238000000354 decomposition reaction Methods 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- 239000001569 carbon dioxide Substances 0.000 description 4
- 229910002092 carbon dioxide Inorganic materials 0.000 description 4
- 238000003988 headspace gas chromatography Methods 0.000 description 4
- 239000003960 organic solvent Substances 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 206010008428 Chemical poisoning Diseases 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000011109 contamination Methods 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000000691 measurement method Methods 0.000 description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 2
- 230000002265 prevention Effects 0.000 description 2
- 238000011002 quantification Methods 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 230000002485 urinary effect Effects 0.000 description 2
- VZSRBBMJRBPUNF-UHFFFAOYSA-N 2-(2,3-dihydro-1H-inden-2-ylamino)-N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]pyrimidine-5-carboxamide Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C(=O)NCCC(N1CC2=C(CC1)NN=N2)=O VZSRBBMJRBPUNF-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- CYTYCFOTNPOANT-UHFFFAOYSA-N Perchloroethylene Chemical group ClC(Cl)=C(Cl)Cl CYTYCFOTNPOANT-UHFFFAOYSA-N 0.000 description 1
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical group ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005264 electron capture Effects 0.000 description 1
- 230000032050 esterification Effects 0.000 description 1
- 239000012374 esterification agent Substances 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 239000008235 industrial water Substances 0.000 description 1
- 239000002207 metabolite Substances 0.000 description 1
- VHFUHRXYRYWELT-UHFFFAOYSA-N methyl 2,2,2-trichloroacetate Chemical compound COC(=O)C(Cl)(Cl)Cl VHFUHRXYRYWELT-UHFFFAOYSA-N 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229950011008 tetrachloroethylene Drugs 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- ZBZJXHCVGLJWFG-UHFFFAOYSA-N trichloromethyl(.) Chemical compound Cl[C](Cl)Cl ZBZJXHCVGLJWFG-UHFFFAOYSA-N 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Abstract
Description
【発明の詳細な説明】
［発明の目的］
（産業上の利用分野）
本発明は、ヒトの尿のような水を主成分とする物質中の
トリクロロ酢酸の濃度を測定する方法に関する。DETAILED DESCRIPTION OF THE INVENTION [Object of the Invention] (Industrial Application Field) The present invention relates to a method for measuring the concentration of trichloroacetic acid in a water-based substance such as human urine.
（従来の技術）
近年、トリクロロエチレン、テトラクロロエチレン、１
，１．１−トリクロロエタンなどの有機塩素系溶剤の人
体に対する有害性か問題になっている。(Prior art) In recent years, trichlorethylene, tetrachlorethylene,
, 1. The toxicity of organic chlorine solvents such as 1-trichloroethane to the human body has become a problem.
このため、たとえば平成元年１０月改正の有機溶剤中毒
予防規則（労働省令第３６号）において、事業主に対し
、上記３種の有機溶剤を取り扱う作業者についての健康
管理を義務づけてイル。For this reason, for example, the Organic Solvent Poisoning Prevention Ordinance (Ministry of Labor Ordinance No. 36) revised in October 1989 requires business owners to manage the health of workers who handle the three types of organic solvents mentioned above.
ところで、これら溶剤類の排水や用水中の濃度は、たと
えば、ＪＩＳ Ｋ ０１２５に示されたヘッドスペース
・ガスクロマトグラフ法によって容易に測定することが
できるが、人体に取り込まれた溶剤類の濃度は直接測定
することか不可能である。そこて通常は、尿に混じって
排出される代謝物の濃度から、体内汚染の程度を推定し
ている。すなわち、たとえば上記３種の溶剤の場合、体
内に入るといずれもトリクロロ酢酸に変化して尿中に排
出されることから、このトリクロロ酢酸の尿中濃度を測
定することにより、各溶剤の体内汚染の程度を推定して
いる。ちなみに上述の有機溶剤中毒予防規則において、
このトリクロロ酢酸の尿中濃度の測定を、上記３種の有
機溶剤に対する臨床検査項目としてあげている。 ゛
このような状況の中から、トリクロロ酢酸の尿中濃度の
測定の需要が昨今急激に増加しているが、従来、この測
定には、次のような方法が用いられてきた。Incidentally, the concentration of these solvents in waste water and industrial water can be easily measured, for example, by the headspace gas chromatography method specified in JIS K 0125, but the concentration of solvents taken into the human body cannot be measured directly. It is impossible to measure. Therefore, the degree of internal contamination is usually estimated from the concentration of metabolites excreted in urine. In other words, for example, in the case of the three types of solvents mentioned above, when they enter the body, they all change to trichloroacetic acid and are excreted in the urine, so by measuring the concentration of trichloroacetic acid in the urine, it is possible to determine the internal contamination of each solvent. The extent of this is estimated. By the way, in the organic solvent poisoning prevention regulations mentioned above,
Measurement of the urinary concentration of trichloroacetic acid is listed as a clinical test item for the three types of organic solvents mentioned above. ``Under these circumstances, the demand for measuring the urinary concentration of trichloroacetic acid has increased rapidly in recent years. Conventionally, the following methods have been used for this measurement.
すなわち、前述したようにヘッドスペース・ガスクロマ
トグラフ法は、水溶液中の、水に溶解しにくい微量の揮
発性液体（または気体）物質の濃度を測定する技術で、
空気と共に密封された試料水溶液に含まれる水に溶は難
い液体（または気体）物質が、水溶液中から徐々に空気
中に抜は出し大幅に濃縮されて平衡に達することを利用
して、その空気層（ヘッドスペース）中の濃度を測定す
ることによりもとの水溶液中の濃度を求めようとす′る
もので、感度の高い測定方法として知られている。一方
、トリクロロ酢酸は水に非常に溶けやすく、常温では固
体である。そこで、試料に硫酸とメタノールを主成分と
する薬品（エステル化剤）を加えて試料中のトリクロロ
酢酸を次式に示すようにメチルエステル化し、揮発性の
高いトリクロロ酢酸メチルを生成させ、この物質の濃度
を上記ヘッドスペース・ガスクロマトグラフ法で測定す
ることにより、もとの試料中に存在していたトリクロロ
酢酸の濃度を求めていた。In other words, as mentioned above, headspace gas chromatography is a technology that measures the concentration of minute amounts of volatile liquid (or gas) substances that are difficult to dissolve in water in an aqueous solution.
Taking advantage of the fact that liquid (or gas) substances that are difficult to dissolve in water and are contained in a sample aqueous solution sealed together with air are gradually expelled from the aqueous solution into the air and are greatly concentrated and reach equilibrium, the air is This method attempts to determine the concentration in the original aqueous solution by measuring the concentration in the layer (headspace), and is known as a highly sensitive measurement method. On the other hand, trichloroacetic acid is highly soluble in water and is solid at room temperature. Therefore, a chemical (esterifying agent) whose main components are sulfuric acid and methanol is added to the sample to methyl esterify the trichloroacetic acid in the sample as shown in the following formula, producing highly volatile methyl trichloroacetate. The concentration of trichloroacetic acid present in the original sample was determined by measuring the concentration of trichloroacetic acid using the headspace gas chromatography method described above.
ＣＣ１３Ｃ０ＯＨ＋ＣＨｉ ０Ｈ＝ＣＣＨ３ＣＯＯＣＨ
３＋Ｈ２０しかしながら、このような従来の技術には以
下のような問題点がある。CC13C0OH+CHi 0H=CCH3COOCH
3+H20 However, such conventional technology has the following problems.
まず、危険な硫酸や有毒なメタノールを含む薬品（エス
テル化剤）を使用しなければならない。First, chemicals (esterifying agents) must be used, including dangerous sulfuric acid and toxic methanol.
また、エステル化剤とトリクロロ酢酸の反応に時間がか
かる（約３０分）ため、測定に長時間を要する。さらに
エステル化剤を加えた分だけ試料がうすめられることに
なり、測定感度が低下する。Furthermore, since the reaction between the esterification agent and trichloroacetic acid takes time (approximately 30 minutes), the measurement takes a long time. Furthermore, the sample is diluted by the addition of the esterifying agent, resulting in a decrease in measurement sensitivity.
（発明が解決しようとする課題）
このように、トリクロロ酢酸の尿中の濃度測定の需要が
増加しているが、従来のトリクロロ酢酸をメチルエステ
ル化してヘッドスペース・ガスクロマトグラフ法により
測定する方法では、安全面に問題があり、また測定に時
間がかかり、測定感度も低いなどの問題があった。(Problems to be Solved by the Invention) As described above, there is an increasing demand for measuring the concentration of trichloroacetic acid in urine, but the conventional method of measuring trichloroacetic acid by methyl esterification and headspace gas chromatography is not possible. However, there were other problems such as safety, time-consuming measurement, and low measurement sensitivity.
本発明はこのような従来技術の課題を解決するためにな
されたもので、尿のような水を主成分とする物質中のト
リクロロ酢酸の濃度を安全かつ短時間に測定することが
でき、しかも感度も高いトリクロロ酢酸の濃度測定方法
を提供することを目的とする。The present invention was made to solve the problems of the prior art, and it is possible to safely and quickly measure the concentration of trichloroacetic acid in a substance whose main component is water, such as urine. The purpose of the present invention is to provide a method for measuring the concentration of trichloroacetic acid with high sensitivity.
［発明の構成］
（課題を解決するための手段）
本発明は、水を主成分とする物質中のトリクロロ酢酸の
濃度を測定するにあたり、
測定試料を空気と共に気密容器内に封入し、この気密容
器を８０℃以上にまで加熱した後、前記気密容器内の気
相の組成をガスクロマトグラフィーにより分析して前記
気相中に含まれるクロロホルム量を求め、このクロロホ
ルム量に基づいてトリクロロ酢酸の水を主成分とする物
質中における濃度を算出することを特徴としている。[Structure of the Invention] (Means for Solving the Problems) In the present invention, when measuring the concentration of trichloroacetic acid in a substance whose main component is water, the measurement sample is sealed together with air in an airtight container, and the airtight container is sealed. After heating the container to 80°C or higher, the composition of the gas phase in the airtight container is analyzed by gas chromatography to determine the amount of chloroform contained in the gas phase, and based on this amount of chloroform, the water of trichloroacetic acid is It is characterized by calculating the concentration in a substance whose main component is
以下、本発明方法の原理を説明する。The principle of the method of the present invention will be explained below.
すなわち、測定試料を空気と共に封入した気密容器を８
０℃以上にまで加熱することにより、測定試料中にトリ
クロロ酢酸が含まれる場合に、このトリクロロ酢酸か次
式に示すように速やかに分解し、定量的にクロロホルム
と炭酸ガスを生成する。In other words, an airtight container in which the measurement sample is sealed together with air is
By heating to 0° C. or higher, if trichloroacetic acid is contained in the measurement sample, this trichloroacetic acid is rapidly decomposed as shown in the following formula, and chloroform and carbon dioxide gas are quantitatively produced.
ＣＣｌ３ Ｃ００Ｈ＝ＣＨＣ１３＋ｃｏ□ ・・
・ ［Ｉ］生成したクロロホルムおよび炭酸ガスのうち
、クロロホルムは水に溶けにくい揮発性の液体であるた
め、気密容器内の空気中に徐々に抜は出し、濃縮されて
平衡に達する。したがって、この後、気密容器内の気相
の組成をガスクロマトグラフィーにより分析することに
より、気相中のクロロホルム量を求めることができ、こ
のクロロホルム量をトリクロロ酢酸量に換算し、その値
を測定試料量で除すことにより、測定試料中のトリクロ
ロ酢酸の濃度を求めることができる。CCl3 C00H=CHC13+co□...
- [I] Among the chloroform and carbon dioxide gases produced, chloroform is a volatile liquid that is difficult to dissolve in water, so it is gradually released into the air in an airtight container and concentrated to reach equilibrium. Therefore, by analyzing the composition of the gas phase inside the airtight container by gas chromatography, the amount of chloroform in the gas phase can be determined.The amount of chloroform is converted into the amount of trichloroacetic acid, and the value is measured. By dividing by the sample amount, the concentration of trichloroacetic acid in the measurement sample can be determined.
本発明において、測定試料を空気と共に封入した気密容
器の８０℃以上としたのは、８０℃未満ではトリクロロ
酢酸のクロロホルムと炭酸ガスへの分解速度が非常に遅
く測定に時間がかかるばかりか、分解か十分進まずに測
定値が不正確になるおそれがあるからである。ただしあ
まり高いと、分解速度は速くなるものの、内部圧力が上
昇して気密容器が破裂する危険が生じる。したがって、
加熱温度は、分解速度とともに、容器の耐圧性、これに
ともなうコストの上昇を考慮して定めることが望ましく
、９０〜１２０℃の範囲がより好ましい。In the present invention, the temperature of the airtight container in which the measurement sample is sealed together with air is set at 80°C or higher.If the temperature is lower than 80°C, the rate of decomposition of trichloroacetic acid into chloroform and carbon dioxide gas is very slow, and not only does it take a long time to measure, but it also decomposes. This is because there is a risk that the measurement value will not be accurate enough. However, if the temperature is too high, although the decomposition rate will be faster, the internal pressure will increase and there is a risk that the airtight container will burst. therefore,
The heating temperature is desirably determined in consideration of the decomposition rate, the pressure resistance of the container, and the accompanying cost increase, and is more preferably in the range of 90 to 120°C.
ちなみに、図面に示したグラフは、トリクロロ酢酸を熱
分解したときの加熱温度および加熱時間に対する分解生
成物（クロロホルム）の回収率を示したものである。Incidentally, the graph shown in the drawing shows the recovery rate of the decomposition product (chloroform) with respect to the heating temperature and heating time when trichloroacetic acid is thermally decomposed.
（作 用）
本発明方法においては、測定試料を空気と共に封入した
気密容器を８０℃以上にまで加熱することにより、測定
試料中に含まれるトリクロロ酢酸をクロロホルムと炭酸
ガスに分解し、ここで生成されたクロロホルムをその性
質を利用して気密容器内の気相中に移行させガスクロマ
トグラフィーにより分析して求めるので、薬品は全く必
要とせず、従来のトリクロロ酢酸をメチルエステル化し
て測定する方法に比べてはるかに安全であり、感度が低
下することもない。しかも、トリクロロ酢酸の熱分解は
８０℃以上の加熱により速やかに進行するため、短時間
の測定が可能である。さらに特別な装置を必要としない
ので経済性の面でも良好である。(Function) In the method of the present invention, trichloroacetic acid contained in the measurement sample is decomposed into chloroform and carbon dioxide gas by heating an airtight container in which the measurement sample is sealed together with air to 80°C or higher. Taking advantage of its properties, the chloroform is transferred into the gas phase in an airtight container and analyzed using gas chromatography.Therefore, no chemicals are required, and this method replaces the conventional measurement method of converting trichloroacetic acid into methyl ester. It is much safer and does not reduce sensitivity. Moreover, since the thermal decomposition of trichloroacetic acid proceeds rapidly by heating at 80° C. or higher, measurement can be carried out in a short time. Furthermore, since no special equipment is required, it is also economical.
（実施例） 以下、本発明の実施例を記載する。(Example) Examples of the present invention will be described below.
実施例１
ヒトの尿１ｍＪ２を、気密性の４ｍｇスクリューキャッ
プバイアルビンに採り密栓した。次いて、この容器を８
０℃の湯浴中に浸漬し １２０分間加熱した後、２５℃
の水浴中に１０分間保持した。Example 1 1 mJ2 of human urine was collected into an airtight 4 mg screw cap vial and the vial was tightly stoppered. Next, add this container to 8
After immersing in a 0°C water bath and heating for 120 minutes, it was heated to 25°C.
was kept in a water bath for 10 minutes.
この後、容器内の気相５０μｇをガスタイトシリンジで
採取し、ＥＣＤ （電子捕獲型）検出器を備えたガスク
ロマトグラフでその中に含まれるクロロホルムの量を測
定した。ここで得られたクロロホルムの量を前記［Ｉ］
式に基づく化学量論的計算により、トリクロロ酢酸量に
換算し、それを測定に使用した尿量で除して濃度を求め
た。Thereafter, 50 μg of the gas phase in the container was collected using a gas tight syringe, and the amount of chloroform contained therein was measured using a gas chromatograph equipped with an ECD (electron capture type) detector. The amount of chloroform obtained here is the amount of [I]
The concentration was determined by converting the amount of trichloroacetic acid into the amount of trichloroacetic acid by stoichiometric calculation based on the formula and dividing it by the amount of urine used for measurement.
この実施例の定量下限濃度および１個の試料の測定に要
した時間は、表に示した通り、それぞれ０．０４μｇ／
ｍＤおよび１４０分間であった。As shown in the table, the lower limit of quantitation concentration and the time required for measuring one sample in this example were 0.04 μg/
mD and 140 minutes.
実施例２〜４
ヒトの尿を採取した４ｍ１ｌスクリユーキヤツプバイア
ルビンを加熱する湯浴温度および時間を、９０℃で２０
分（実施例２） 、１１０℃で１０分（実施例３）、１
２０℃で５分（実施例４）とした点を除いてそれぞれ実
施例１の場合と同様にして、尿中のトリクロロ酢酸濃度
を求めた。Examples 2 to 4 The temperature and time of a hot water bath for heating a 4 ml screw cap vial in which human urine was collected was set at 90°C for 20 min.
min (Example 2), 10 min at 110°C (Example 3), 1
The concentration of trichloroacetic acid in urine was determined in the same manner as in Example 1, except that the temperature was 20° C. for 5 minutes (Example 4).
各実施例の定量下限濃度と １個の試料の測定に要した
時間は表に示した通りであった。The lower limit of quantitation concentration and the time required for measurement of one sample for each example were as shown in the table.
実施例５
ヒトの尿５ｍＮを、気密性の２０ｍ （ｌアルミシール
バイアルビンに採取した点、および、この容器を加熱す
る湯浴温度および時間を１１０℃で２０分間とした点を
除いて、実施例１の場合と同様にして尿中のトリクロロ
酢酸濃度を求めた。Example 5 The procedure was carried out with the exception that 5 mN of human urine was collected in an airtight 20 m aluminum sealed vial, and that the water bath temperature and time for heating the container were 110° C. for 20 minutes. Trichloroacetic acid concentration in urine was determined in the same manner as in Example 1.
この実施例の定量下限濃度と １個の試料の測定に要し
た時間は表に示した通りであった〇実施例６
ヒトの尿０．５ｍ Ｍを、気密性の２ｍ１）スクリュー
キャップバイアルビンに採取した点を除いて、実施例３
の場合と同様にして尿中のトリクロロ酢酸濃度を求めた
。The lower limit of quantitation concentration in this example and the time required for measuring one sample were as shown in the table. Example 6 0.5 mM of human urine was placed in an airtight 2 m screw cap vial. Example 3, except for the points taken.
Trichloroacetic acid concentration in urine was determined in the same manner as in the case of .
この実施例の定量下限濃度と １個の試料の測定に要し
た時間は表に示した通りであった。The lower limit of quantitation concentration and the time required for measurement of one sample in this example are shown in the table.
比較例
ヒトの尿を採取した４ｍｊ）スクリューキャップバイア
ルビンを加熱する湯浴温度および時間を、７０℃で１２
０分とした点を除いて実施例１の場合と同様にして、尿
中のトリクロロ酢酸濃度を求めた。Comparative Example Human urine was collected 4mj) The water bath temperature and time for heating the screw cap vial were heated to 70°C for 12
The trichloroacetic acid concentration in urine was determined in the same manner as in Example 1 except that the time was 0 minutes.
この比較例の定量下限濃度と １個の試料の測定に要し
た時間は表に示した通りであった。The lower limit of quantification concentration and the time required for measurement of one sample in this comparative example were as shown in the table.
（以下余白）
なお、従来のトリクロロ酢酸をメチルエステル化して測
定する方法による定量下限濃度は０．４μｇ／ｍＮであ
り、測定時間は６０分以上を要する。(Left below) Note that the lower limit concentration of quantification by the conventional method of measuring by converting trichloroacetic acid into methyl ester is 0.4 μg/mN, and the measurement time requires 60 minutes or more.
［発明の効果］
以上説明したように、本発明方法によれば、トリクロロ
酢酸を熱分解し、これにより生ずるクロロホルムをガス
クロマトグラフィーにより分析して求めるので、薬品は
全く必要とせず、従来のトリクロロ酢酸をメチルエステ
ル化して測定する方法に比べてはるかに安全であり、感
度が低下することもない。しかも、トリクロロ酢酸の熱
分解は８０℃以上の加熱により速やかに進行するため、
短時間の測定が可能である。さらに特別な装置を必要と
しないので経済性にも優れている。[Effects of the Invention] As explained above, according to the method of the present invention, trichloroacetic acid is thermally decomposed and the resulting chloroform is analyzed and determined by gas chromatography. It is much safer than the method of measuring by converting acetic acid into methyl ester, and there is no decrease in sensitivity. Moreover, the thermal decomposition of trichloroacetic acid proceeds rapidly when heated above 80°C.
Short-time measurements are possible. Furthermore, since no special equipment is required, it is also economical.
第１図はトリクロロ酢酸を熱分解したときの加熱温度お
よび加熱時間に対する分解生成物（クロロホルム）の回
収率を示した図である。
出願人 株式会社 東芝
代理人 弁理士 須 山 佐 −FIG. 1 is a diagram showing the recovery rate of a decomposition product (chloroform) with respect to heating temperature and heating time when trichloroacetic acid is thermally decomposed. Applicant Toshiba Corporation Representative Patent Attorney Sasa Suyama −
Claims (1)
を測定するにあたり、 測定試料を空気と共に気密容器内に封入し、この気密容
器を８０℃以上にまで加熱した後、前記気密容器内の気
相の組成をガスクロマトグラフィーにより分析して前記
気相中に含まれるクロロホルムの量を求め、このクロロ
ホルム量に基づいてトリクロロ酢酸の水を主成分とする
物質中における濃度を算出することを特徴とするトリク
ロロ酢酸の濃度測定方法。(1) When measuring the concentration of trichloroacetic acid in a substance whose main component is water, the measurement sample is sealed in an airtight container with air, and after heating this airtight container to 80°C or higher, the sample is placed inside the airtight container. The composition of the gas phase is analyzed by gas chromatography to determine the amount of chloroform contained in the gas phase, and the concentration of trichloroacetic acid in a substance whose main component is water is calculated based on the amount of chloroform. Characteristic method for measuring the concentration of trichloroacetic acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP32712990A JPH04194751A (en) | 1990-11-28 | 1990-11-28 | Measuring method of concentration of trichloroacetic acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP32712990A JPH04194751A (en) | 1990-11-28 | 1990-11-28 | Measuring method of concentration of trichloroacetic acid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH04194751A true JPH04194751A (en) | 1992-07-14 |
Family
ID=18195636
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP32712990A Pending JPH04194751A (en) | 1990-11-28 | 1990-11-28 | Measuring method of concentration of trichloroacetic acid |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH04194751A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107422053A (en) * | 2017-07-04 | 2017-12-01 | 苏州出入境检验检疫局检验检疫综合技术中心 | A kind of method of trichloroacetic acid in LC-MS detection cosmetics |
-
1990
- 1990-11-28 JP JP32712990A patent/JPH04194751A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107422053A (en) * | 2017-07-04 | 2017-12-01 | 苏州出入境检验检疫局检验检疫综合技术中心 | A kind of method of trichloroacetic acid in LC-MS detection cosmetics |
| CN107422053B (en) * | 2017-07-04 | 2020-08-21 | 苏州出入境检验检疫局检验检疫综合技术中心 | Method for detecting trichloroacetic acid in cosmetics by liquid chromatography-mass spectrometry |
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