역상 액체 크로마토그래피에서 이동상 조성의 함수로서 taxol의 분리도

정용안; 정성택; 노경호

HWAHAK KONGHAK, Vol.35, No.5, 712-716, October, 1997

Export Citation

역상 액체 크로마토그래피에서 이동상 조성의 함수로서 taxol의 분리도

Resolution of Taxol in Terms of Mobile Phase Compositions in RP-HPLC

정용안, 정성택, 노경호

초록

역상 액체크로마토그래피와 물, 아세토나이트릴, 메탄올의 3성분계 이동상을 사용하여 주목나무 추출물에 포함된 taxol을 체류거동이 비슷한 cephalomannine, 10-deacetyltaxol로부터 분리하였다. 물을 기본으로 유기용매인 아세토나이트릴과 메탄올의 이동상의 조성율 5%씩 변화시켜서 15번의 실험을 수행하여 cephalomannine과 taxol, taxol과 10-deacetyltaxol의 분리도를 측정하였다. 이 실험결과로부터 각기의 분리도를 이동상 조성의 함수로서 표시된 실험상관식을 구하였다. 실험값에 가장 잘 일치하는 상관식에는 각기 조성의 선형성과 상호관련항이 포함되었다. 이 실험상관식으로부터 이동상의 최적 범위를 분리도와 분리시간을 기준으로 정하였고 이 중에 포함된 56/39/5 (물/아세토나이트릴/메탄올, vol.%)에서 주목나무로부터 얻어진 추출물을 분리한 결과 실험상관식으로부터 계산한 분리도와 잘 일치하였다.

The separation of taxol from cephalomannine and 10-deacetyltaxol, in extract from yew trees was studied by an isocratic reversed-phase high performance liquid chromatography(RP-HPLC) with the mobile phase consisted of water, acetonitrile, and methanol. The compositions in mobile phase were varied to an increment of 5% of acetonitrile and/or methanol and the resolutions of cephalomannine/taxol and taxol/10-deacetyltaxol were measured by fifteen experimental runs. Using the experimental results, each resolution was fitted to the correlation equation as a function of mobile phase composition. The best correlation equation contained the linear and interaction terms of mobile phase composition. The optimized range for the resolution of the three components was determined by the resolution and separation time. The extraction from yew tree was separated with the mobile phase composition of 56/39/5(water/acetonitrile/methanol, vol.%) in the optimized range. The calculated resolution from the correlation equation was in good agreement with the experimental one.

Keywords:Taxol;Mobile Phase;Resolution;HPLC

[References]

Berridge JC, "Techniques for the Automated Optimization of HPLC Separation," Wiley-Interscience, New York (1985)
Ravanat JL, Douki T, Incardona MF, Cadet J, J. Liq. Chromatogr., 16, 3185 (1993)
Chye PO, Chow KK, Choon LN, Fei MO, J. Chromatogr. A, 692, 207 (1995)
Hamilton RJ, Sewell PA, "Introduction to High Performance Liquid Chromatography," 2nd Ed., 13 (1982)
Hancock WS, Rosanne CC, Kirkland JJ, Snyder LR, J. Chromatogr. A, 686, 31 (1994)
Guillaume Y, Guinchard C, J. Liq. Chromatogr., 17, 1443 (1994)
Clajch JL, Kirkland JJ, Snyder LR, J. Chromatogr., 238, 269 (1982)
Shen HX, Yang GS, Gao RY, Wang QS, Chromatographia, 40, 303 (1995)
Wolff ME, "Burger's Medicinal Chemistry and Drug Discovery," 5th Ed., John Wiley & Sons, NY, U.S.A., 996 (1995)
Witherup KM, Look SA, Stasko HW, Mccloud TG, Muschik HJ, J. Liq. Chromatogr., 12, 2117 (1989)
Kappakva V, Rao R, Bhakuni JJ, Richard MD, J. Liq. Chromatogr. REL. Technol., 19(3), 427 (1996)
Valiente BA, Duprat F, J. Liq. Chromatogr., 17, 1709 (1994)
Nina H, Fred B, Fred M, Miner M, "Basic Liquid Chromatography," Varian Aerograph (1971)

[Referenced By]

[1] Berridge JC, "Techniques for the Automated Optimization of HPLC Separation," Wiley-Interscience, New York (1985)

[2] Ravanat JL, Douki T, Incardona MF, Cadet J, J. Liq. Chromatogr., 16, 3185 (1993)

[3] Chye PO, Chow KK, Choon LN, Fei MO, J. Chromatogr. A, 692, 207 (1995)

[4] Hamilton RJ, Sewell PA, "Introduction to High Performance Liquid Chromatography," 2nd Ed., 13 (1982)

[5] Hancock WS, Rosanne CC, Kirkland JJ, Snyder LR, J. Chromatogr. A, 686, 31 (1994)

[6] Guillaume Y, Guinchard C, J. Liq. Chromatogr., 17, 1443 (1994)

[7] Clajch JL, Kirkland JJ, Snyder LR, J. Chromatogr., 238, 269 (1982)

[8] Shen HX, Yang GS, Gao RY, Wang QS, Chromatographia, 40, 303 (1995)

[9] Wolff ME, "Burger's Medicinal Chemistry and Drug Discovery," 5th Ed., John Wiley & Sons, NY, U.S.A., 996 (1995)

[10] Witherup KM, Look SA, Stasko HW, Mccloud TG, Muschik HJ, J. Liq. Chromatogr., 12, 2117 (1989)

[11] Kappakva V, Rao R, Bhakuni JJ, Richard MD, J. Liq. Chromatogr. REL. Technol., 19(3), 427 (1996)

[12] Valiente BA, Duprat F, J. Liq. Chromatogr., 17, 1709 (1994)

[13] Nina H, Fred B, Fred M, Miner M, "Basic Liquid Chromatography," Varian Aerograph (1971)