藏药榜嘎中的双酯型和内酯型生物碱分析方法研究

目的建立藏药榜嘎中双酯型和内酯型生物碱的测定方法,为榜嘎的质量标准提高提供参考。方法采用高效液相色谱法。色谱柱为:Phenomenes luna C18(250mm×4.6mm,5μm);流速:1.0mL·min-1。双酯型生物碱的流动相为:A为乙腈-四氢呋喃(25∶15),B为0.1mol·L-1醋酸铵溶液(每1 000mL加冰乙酸0.5mL),梯度洗脱;检测波长为235nm;柱温为室温。内酯型生物碱的流动相为甲醇-水-氯仿-三乙胺(70∶30∶2∶0.1);检测波长230nm;柱温30℃。结果榜嘎中均不含新乌头碱、乌头碱、次乌头碱等双酯型生物碱;内酯型生物碱:阿替新在2.024²0.24μg范围内线性关系良好,线性方程:Y=1.918×104 X-678(r=0.999 9),平均回收率97.3%,RSD=0.9%;异叶乌头碱在2.00820.24μg范围内线性关系良好,线性方程:Y=1.918×104 X-678(r=0.999 9),平均回收率97.3%,RSD=0.9%;异叶乌头碱在2.008²0.08μg范围内线性关系良好,线性方程:Y=1.602×104 X-215(r=0.999 9),平均回收率98.6%,RSD=1.4%。结论该方法准确,可靠,专属性强,可用于榜嘎的质量控制。

Study on the analytical method of diester-type and lactone-type alkaloids in Tibetan medicine Bangga

Objective To establish an HPLC method for the determination of diester-type and lactone-type alkaloids in Bangga （a Tibetan traditional medicine） .Methods The column was Phenomenex luna C18 （250 mm × 4 .6 mm ,5 μm） ,and the flow rate was 1 .0 mL · min-1 .The diester-type mobile phase was A acetonitrile-tetrahydrofuran （25∶15） ,B 0 .1 mol · L -1 ammonium acetate solution （add 0 .5 mL glacial acetic acid per 1 000 mL） ,gradient elution ,the detection wavelength was 235 nm ,and the column temperature was at room temperature .The lactone-type mobile phase was methanol-water-chloroform-triethylamine （70∶30∶2∶0 .1） .The flow rate was 1 .0 mL · min-1 ,the detection wavelength was 230 nm ,and the column temperature was at 35 ℃ .Re-sults There is no double that ester alkaloids such as aconitine ,new aconitine ,and hypaconitine exist in Bangga .The linearity range of atisine was 2 .024-20 .24μg ,Y=1 .918 × 104 X-678（r=0 .999 9） ,and the average recovery was 97 .3% ,RSD=0 .9% ;The lin-earity range of hetisine was 2 .008-20 .08 μg ,Y=1 .602 × 104 X -215（r=0 .999 9） ,and the average recovery was 98 .6% ,RSD=1 .4% .Conclusion The method is accurate ,reliable and specific .It could be used for the quality control of Bangga .