Analytical Science and Technology (분석과학)

The Korean Society of Analytical Sciences (한국분석과학회)
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Development and validation of a HPLC method for the simultaneous determination of chlorquinaldol and promestriene in complex prescription

복방제제 내 클로르퀴날돌과 프로메스트리엔에 대한 HPLC 기반 동시분석법의 개발 및 밸리데이션

  • Lee, Seul-Ji (College of Pharmacy and Research Institute of Pharmaceutical Sciences, Seoul National University) ;
  • Shin, Sang-Yeon (College of Pharmacy and Research Institute of Pharmaceutical Sciences, Seoul National University) ;
  • Shin, Hae-Jin (College of Pharmacy and Research Institute of Pharmaceutical Sciences, Seoul National University) ;
  • Lee, Jin-Gyun (College of Pharmacy and Research Institute of Pharmaceutical Sciences, Seoul National University) ;
  • Kim, Dong-Hwan (Pharmaceutical Standardization Research and Testing Division, Korea Food & Drug Administration) ;
  • Lee, Su-Jung (Pharmaceutical Standardization Research and Testing Division, Korea Food & Drug Administration) ;
  • Han, Sang-Beom (Dept. of Pharmaceutical Analysis, College of Pharmacy, Chung-Ang University) ;
  • Park, Jeong-Hill (College of Pharmacy and Research Institute of Pharmaceutical Sciences, Seoul National University) ;
  • Lee, Jeong-Mi (School of Pharmacy, Sungkyunkwan University) ;
  • Kwon, Sung-Won (College of Pharmacy and Research Institute of Pharmaceutical Sciences, Seoul National University)
  • Received : 2012.01.10
  • Accepted : 2012.02.17
  • Published : 2012.04.25
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Abstract

Currently, many types of compound preparations are being used but the quality control guidelines for their use are lacking. In case of single compound drug, the quality control methods are specified in the pharmacopeia. However, there is no method to simultaneously analyze compound preparations. In this study, a simple validated analytical method for HPLC separation of chlorquinaldol and promestriene is introduced. Validation was divided into categories including linearity, precision, accuracy (recovery) and system suitability. The contents of the products which are on the market were monitored using the validated analytical method and the robustness of the analytical method was tested by conducting an inter-laboratory validation.

현재 시중에 많은 복방제제가 유통되고 있음에도 불구하고 이의 품질관리를 위한 시험법은 부족한 실정이다. 여러 주효 성분을 가지는 복방제제의 경우 대부분 약전에 수재된 항목 중 2개 이상의 조합으로 구성되어 있으나 약전에 단일 항목에 대한 시험법이 고시되어 있을 뿐 여러 항목을 한번에 시험하는 방법이 없어 한가지 제제를 관리 하는 데에 여러 시험법이 요구되어 효율이 낮고 비용이 높다. 따라서 본 연구는 현재 유통중인 복방제제의 새로운 분석법을 개발한 과정과 그 때에 적용되는 기준을 제시하고 그 결과를 검증하였다. 복방 프로메스트리엔, 클로르퀴날돌 제제에 대한 새로운 분석법을 HPLC를 기반으로 가장 적용이 용이하게 개발하였으며 직선성, 정밀성, 정확성(회수율), 시스템 적합성(반복성, 분리도) 등의 항목에 대하여 밸리데이션을 수행함으로써 분석법을 검증하였다. 또한 개발된 시험법을 이용하여 시중 제품을 모니터링하고 실험실간 밸리데이션을 수행하여 시험법의 견고성을 확인함으로써 새로운 고시안으로서의 가능성을 제시하였다.

Keywords

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