Analytical Science and Technology (분석과학)

The Korean Society of Analytical Sciences (한국분석과학회)
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1Determination of optical purity of N-acetyl-1-naphthylethylamine by chiral chromatography and NMR spectroscopy

키랄 크로마토그래피와 NMR 분광법에 의한 N-acetyl-1-naphthylethylamine의 광학순도 측정

  • Jeong, Young-Han (Analysis & Evaluation Research Institute, KOLON central research park) ;
  • Ryoo, Jae-Jeong (Dept. of Chemistry Education, Kyungpook National University)
  • 정영한 (코오롱 중앙 연구소 분석센타) ;
  • 류재정 (경북대학교 화학교육과)
  • Received : 2009.10.01
  • Accepted : 2010.01.09
  • Published : 2010.02.25
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Abstract

(R)-N-3,5-dinitrobenzoyl (DNB) phenylglycinol derived chiral selector was used as a HPLC chiral stationary phase (CSP) for the resolution of racemic N-acylnaphthylalkylamines. In this study, determination of optical purity was performed by both chiral chromatography and NMR spectroscopy by using the (R)-phenylglycinol derived chiral selector. The data of accuracy and precision of each optical purity value are calculated from the results of NMR and HPLC experiments by comparing with true value. Average error of the NMR method was +2.2% with average RSD of 4.54%, while that of HPLC method was -3.5% with average RSD of 3.23%.

(R)-N-3,5-dinitrobenzoyl (DNB) phenylglycinol로 부터 만들어진 키랄 선택제가 라세미 Nacylnaphthylalkylamines의 분리에 HPLC 키랄 정지상으로 이용된 바 있다. 본 연구에서는 (R)-phenylglycinol 유도체 키랄 선택제를 이용하여 키랄 크로마토그래피와 NMR 분광법에 의한 광학순도를 측정하였다. NMR과 HPLC 실험결과를 참값과 비교하여 각 광학순도 측정값의 정확도와 정밀도를 계산하였다. NMR 방법의 오차는 +2.2%, 평균 RSD는 4.54% 이었고, HPLC 방법의 오차는 -3.5%, 평균 상대표준편차는 3.23% 이었다.

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References

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