HPLC-ELSD法测定贝母中异甾类生物碱及糖苷类成分的含量(英文)

Simultaneous determination of the major isosteroidal alkaloids and their glucosides in the bulbs of Fritillaria by high performance liquid chromatography coupled with evaporative light scattering detection

目的 建立同时测定贝母中 5种异甾类生物碱———peimissine ,imperialine ,sinpeinineA ,imperialine 3β glucoside和yibeinosideA含量的HPLC分析方法。方法 C1 8柱 ;流动相 :乙腈 水 (含 0 1%二乙胺 ) ;梯度洗脱 ,流速 1 0mL·min- 1 ;检测器 :Alltech 5 0 0蒸发光散射检测器 (ELSD)。结果 线性范围为peimissine 13 1～ 2 88 2mg·L- 1 (r2 =0 9975 ) ,imperialine 3β glucoside 7 7～ 16 9 4 mg·L- 1 (r2 =0 9993) ,yibeinosideA 7 3～ 16 0 6mg·L- 1 (r2 =0 9997) ,imperialine 16 5～ 36 3 0mg·L- 1 (r2 =0 9992 ) ,sinpeinineA 8 7～ 191 4mg·L- 1 (r2 =0 994 2 )。5个化合物的精密度和重现性RSD均 <5 %。结论 本方法简便、有效、可行 ,可用于贝母中 5种异甾类生物碱的含量测定。

Aim To establish an HPLC ELSD method for the simultaneous determination of five major bioactive isosteroidal alkaloids and gluco alkaloids in the bulbs of Fritillaria namely peimissine, imperialine, sinpeinine A, imperialine 3β glucoside and yibeinoside A. Methods A Nova Pak C 18 column (150 mm×3 9 mm ID) was used. The chromatography was carried out with a linear gradient programming. The mobile phase was acetonitrile water (containing 0 1% diethylamine) and the flow rate was 1 0 mL·min -1 . Results The linear range of peimissine was 13 1-288 2 mg·L -1 ( r 2= 0 997 5 ), imperialine 3β glucoside 7 7-169 4 mg·L -1 ( r 2= 0 999 3 ), yibeinoside A 7 3-160 6 mg·L -1 ( r 2= 0 999 7 ), imperialine 16 5-363 0 mg·L -1 ( r 2= 0 999 2 ), sinpeinine A 8 7-191 4 mg·L -1 ( r 2= 0 994 2 ). Conclusion The method is accurate with overall intra and inter day variation less than 5% and recovery more than 95%. The method was successfully applied to analyze five major bioactive alkaloids and gluco alkaloids in three Fritillaria bulbs.