李松林, 李萍, 曾令杰, 李松林. 伊犁贝母中西贝素和西贝素苷的高效液相色谱-蒸发光散射检测法J. 药学学报, 2001, 36(4): 300-302.
引用本文: 李松林, 李萍, 曾令杰, 李松林. 伊犁贝母中西贝素和西贝素苷的高效液相色谱-蒸发光散射检测法J. 药学学报, 2001, 36(4): 300-302.
LI Song-lin, LI Ping, ZHENG Ling-jie, . DETERMINATION OF IMPERIALINE AND IMPERIALINE-3β-D-GLUCOSIDE IN BULBS OF FRITILLARIA PALLIDIFLORA BY HPLC-ELSDJ. Acta Pharmaceutica Sinica, 2001, 36(4): 300-302.
Citation: LI Song-lin, LI Ping, ZHENG Ling-jie, . DETERMINATION OF IMPERIALINE AND IMPERIALINE-3β-D-GLUCOSIDE IN BULBS OF FRITILLARIA PALLIDIFLORA BY HPLC-ELSDJ. Acta Pharmaceutica Sinica, 2001, 36(4): 300-302.

伊犁贝母中西贝素和西贝素苷的高效液相色谱-蒸发光散射检测法

DETERMINATION OF IMPERIALINE AND IMPERIALINE-3β-D-GLUCOSIDE IN BULBS OF FRITILLARIA PALLIDIFLORA BY HPLC-ELSD

  • 摘要: 目的建立伊犁贝母中无紫外吸收的活性异甾体生物碱西贝素和西贝素苷的HPLC测定方法。方法HPLC-蒸发光散射检测器法。结果西贝素苷和西贝素的线性范围分别为48.72-194.88μg·mL-1和60.72-161.92μg·mL-1;RSD日内0.7%和0.9%,日间1.0%和1.5%;低、中、高浓度回收率分别为95.8%,96.9%,96.0%和97.1%,96.7%,96.8%;最低检测限分别为1.53和2.43μg·mL-1。结论本法快速、简便、灵敏和分离度好,适用于伊贝母中活性生物碱的测定。

     

    Abstract: AIM To establish an HPLC (high performance liquid chromatography)-ELSD (evaporative light scattering detector) method for the quantification of chromophore-lacking imperialine (I) and imperialine-3β-D-glucoside (II) in bulbs of Fritillaria pallidiflora. METHODS By optimizing the chromatographic conditions of HPLC and the parameters of ELSD to test the methodology. Column: Kromasil C-18 (5 μm, 200 mm×4.6 mm), mobile phase: acetonitrile-water-triethylamine (71∶29∶0.03), flow rate: 1.0 mL*min-1, drift tube temperature: 88℃, gas flow-rate: 2.38 L·min-1. RESULTS The calibration curves were linear in the range of 60.72-161.92 μg·mL-1 for I and 48.72-194.88 μg·mL-1 for II. The precisions (RSD) of intra-day and inter-day were less than 1% for I and II. The recoveries of the amounts of 24.28, 30.35 and 36.42 μg for I were 97.1%, 96.6% and 96.8%, and 24.20, 30.24 and 36.29 μg for II were 95.8%, 96.9% and 96.0%. The minimal detectable concentrations of I and II were 2.43 and 1.53 μg·mL-1 respectively. CONCLUSION The established method is simple, rapid, accurate and sensitive, and can be utilized to determine the contents of imperialine and imperialine-3β-D-glucoside in crude drug Yibeimu (derived from the bulbs of Fritillaria pallidiflora).

     

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