附子煎煮过程中酯型生物碱含量的动态变化

Study on Dynamic Variation Patterns of Ester Alkaloids in Radix Aconite Lateralis at Different Decocting Time

目的:研究附子煎煮过程中酯型生物碱的动态变化规律,建立其含量变化与煎煮时间的关系。方法:采用E-clipse XDB C18(4.6 mm×250 mm,5μm)色谱柱,0.1 mol.L-1醋酸铵溶液(每1 000 mL加0.5 mL冰醋酸)为A相,乙腈-四氢呋喃(25∶15)为B相,梯度洗脱,测定生附子和白附片不同时间水煎液中酯型生物碱的含量。结果:生附子中双酯型生物碱水煎极不稳定,仅在0.5 h检测出次乌头碱;而白附片水煎液在10 h内均能检出新乌头碱和次乌头碱,其含量逐渐降低,在4 h内可检出乌头碱。生附子水煎液中3种单酯型生物碱含量呈现逐渐增加的变化趋势,在8 h达到峰值;而白附片水煎液中苯甲酰新乌头原碱和苯甲酰乌头原碱含量先增后减,约在3～5 h达到峰值,苯甲酰次乌头原碱含量在10 h内逐渐增大至峰值。结论:生附子和白附片煎煮过程中酯型生物碱含量的变化规律不同,总体趋势是双酯型生物碱转化为焦新乌头碱、焦乌头碱、焦次乌头碱和苯甲酰新乌头原碱、苯甲酰乌头原碱、苯甲酰次乌头原碱。

Objective：Study on variation of ester alkaloids and hydrolysate in Radix Aconite Lateralis with the change of decocting time to establish the relationship between the content change and decoeting time. Method：HPLC analysis was performed on a Eclipse XDBC18（4.6mm×250mm,5μm） with 0. 1 mol·L^-1 ammonium acetate （contains 0. 5 mL glacial acetic acid per 1 000 mL, phase A） and acetonitrile-tetrahydrofuran （25： 15, phase B ） as mobile phase. Gradient elution was used to the determination of ester alkaloids in Baifupian and crude aconite roots at different decocting time. Result： The diester-type alkaloids in crude Aconite roots were extremely unstable, and there was only hypaconitine detected in 0.5 hours. But it＇s three kinds of monoester-type alkaloid showed a tendency of increasing gradually with increase of decocting time, and reached the peak at 8 hours. The mesaconitine and hypaconitine in Baifupian were detected in the whole decoction process, but the aconitine did＇t detect after 4 hours of decoction. The benzoylmesaconine and benzoylaconine in Baifupian decocted fluid firstly increased and then decreased, after 3-5 hours reached the peak, while the benzoylhypaconine gradually increased to the peak within 10 hours. Conclusion： In the decoction process, the change of ester alkaloids in crude Aconite roots and Baifupian was significantly different. The general trend is that the diester-type alkaloids in crude Aconite roots and Baifupian have transformed into pymesaconitine, pyraconitine, pyrhypaconitine, benzoylmesaconine, benzoylaconine and benzoylhypaconine.