Analytical Science and Technology (분석과학)

The Korean Society of Analytical Sciences (한국분석과학회)
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Rapid and simultaneous determination of metabolites of organic solvents in human urine by high-performance liquid chromatography using a monolithic column

Monolithic 칼럼을 이용한 뇨 중 유기용매 대사체의 신속한 HPLC 동시 분석

  • Received : 2006.08.23
  • Accepted : 2006.09.18
  • Published : 2006.10.28
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Abstract

A HPLC/UV method was developed and validated for the rapid and simultaneous determination of urinary metabolites of organic solvents, mandelic acid, hippuric acid, phenylglyoxylic acid, ortho-, meta- and para-methylhippuric acid, using a monolithic column. The mobile phase was composed of tetrabutylammonium bromide as ion-pairing reagent with a flow rate of 2.4 mL/min. The total run time was less than 2.5 min for all six analytes. Good linearities were obtained for all the metabolites with correlation coefficients above 0.9993. Intra-day precision, accuracy and inter-day precision was 0.01~7.32%, 83.9~116.3% and 0.01~7.16%, respectively. The method was validated and confirmed by quantification of the quality assurance samples of Industrial Safety and Health Research Institute, Korea Occupational Safety and Health Agency.

본 연구에서는 톨루엔, 크실렌, 스티렌 등의 폭로에 대한 측정지표로써 체내에서 대사되어 뇨로 배설되는 마뇨산, 메틸마뇨산, 만델산과 페닐글리옥실산에 대한 신속한 동시분석법을 개발하였다. 일반 충전형 ODS 칼럼과 달리 빠른 유속에서도 고분리능을 구현할 수 있는 monolithic 칼럼을 사용하였고, 이동상으로는 ion-pairing reagent인 tetrabutylammonium bromide 5.5 g과 potassium phosphate monobasic 1.5 g을 증류수 1 L에 녹인 후, 메탄올 0.6 L와 혼합하여 조제한 것을 사용하였으며, 유속 2.4 mL/min에서 분석한 결과, 6종의 유기용매 대사체들을 2.5분 이내에 검출하였다. 일정 농도 범위 내에서 6종 화합물 모두 검량선의 상관계수($r^2$)가 0.9993 이상으로 양호한 직선성을 나타내었다. 각 화합물별로 5가지 농도에 대하여 하루에 5번 반복 실험하여 구한 일내 정밀성 %C.V.와 정확성은 0.01~7.32%, 83.9~116.3%이고 5일간 반복 실험하여 구한 일간 정밀성 %C.V.는 0.01~7.16%이다. 본 분석법은 뇨 중 유기용매 대사체의 분석에 필요한 충분한 감도와 특이성, 직선성, 정확성 및 정밀성을 가지며, 한국산업안전공단 산하 산업안전보건연구원 직업병연구센터의 정도관리 소변시료를 분석 비교하여 그 신뢰성을 확보하였다.

Keywords

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