金晓, 崔凯荣. 用(+)-FLEC手性试剂自动柱前衍生高效液相色谱法拆分麻黄碱类药物对映体J. 药学学报, 1994, 29(2): 122-127.
引用本文: 金晓, 崔凯荣. 用(+)-FLEC手性试剂自动柱前衍生高效液相色谱法拆分麻黄碱类药物对映体J. 药学学报, 1994, 29(2): 122-127.
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X Jin, KR Cui. RESOLUTION OF THE ENANTIOMIERS OF EPHEDRINES USING (+ )一FLEC CHIRAL DERIVATIZATION AND REVERSED—PHASE LIQUID CHROMATOGRAPHYJ. Acta Pharmaceutica Sinica, 1994, 29(2): 122-127.
Citation: X Jin, KR Cui. RESOLUTION OF THE ENANTIOMIERS OF EPHEDRINES USING (+ )一FLEC CHIRAL DERIVATIZATION AND REVERSED—PHASE LIQUID CHROMATOGRAPHYJ. Acta Pharmaceutica Sinica, 1994, 29(2): 122-127.
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用(+)-FLEC手性试剂自动柱前衍生高效液相色谱法拆分麻黄碱类药物对映体

RESOLUTION OF THE ENANTIOMIERS OF EPHEDRINES USING (+ )一FLEC CHIRAL DERIVATIZATION AND REVERSED—PHASE LIQUID CHROMATOGRAPHY

    摘要
  • 摘要: 报道了以(+)-FLEC作为手性衍生化试剂,用反相高效液相色谱技术分离麻黄碱类药物对映异构体的方法。dl-麻黄碱、dl-伪麻黄碱、dl-去甲麻黄碱、dl-去甲伪麻黄碱先与(+)-FLEC形成衍生物后,经过一ODSHypersil柱分离,以水和乙腈为流动相梯度洗脱.二极管阵列检测器在266nm检测。该法从样品衍生化到最终报告全部自动完成。上述各对对映体均达到基线分离,分离度R均大于1.5,方法灵敏度高,最低检出限达10pmo1,保留时间和峰面积的上现性较好,RSD分别为1.1/和3.0%。

     

    Abstract: An automatic and rapid reversed phase liquid chromatographic method for the resolution of enantiomers of four ephedrines using (+)- FLEC as on-line pre-column chiral derivatizing reagent has been devcloped.After dl-ephedrine,dl-pseudoephedrine,dl-norephedrine and dl-norpseudoephedrine were derivatized with the chiral reagent(+)- FLEC 1-( fluorenyl ) ethylchloroformate ,the resulting diastereomers were separated by using an acetontrile-water gradient elution on an ODS Hypersil column .This method was fully automated from sample derivatization to final report. Four enantiomersof ephedrines were well separated with resolution better that 1.5 . Thesensitivity was 1 0 pmol and reproducibility better than 1.0% RSD for retention time and 3 .0%fopeak area.

     

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