摘要
目的 建立HPLC法测定口服制川乌提取物后大鼠体内乌头类生物碱的方法。方法 用Waters2690@996PAD系统,Halsil100C18柱( 250mm×4 6mmID, 5μm),水甲醇二乙胺( 75∶25∶0 .1 )为流动相,流速0. 9mL·min-1,检测波长240nm。结果 乌头碱在心脏、脾脏、肺脏、肾脏的线性范围: 0 .4 -100μg·mL-1,r分别为0 .997 2, 0 .998 6, 0 .999 3, 0 .999 4;在肝脏的线性范围: 2 -200μg·mL-1,r为0 999 0。次乌头碱在心、肝、脾、肺、肾、脑和脊髓的线性范围: 5-100μg·mL-1,r分别为0. 999 4, 0 .999 7, 0 .999 8, 0. 998 4, 0 .999 8, 0 .999 8和0 999 7。乌头碱及次乌头碱的检测限(S/N=3)为0 .4μg·mL-1。各组织中的回收率:乌头碱为88 .7% -102. 2%,次乌头碱为86. 5% -101. 3%。结论 本法为确证乌头类生物碱的中毒提供了科学有效的依据。
Aim To develop an HPLC method for the determination of Aconitum alkaloids extracted from Radix aconiti preparata in rats. Methods Waters 2690@996 PAD system was used. The analytical column was a Halsil 100 C ~18 column (250 mm×4.6 mm ID, 5 μm). The mobile phase was water, methanol and diethyl amine at the ratio of 75∶25∶0.1. The flow rate was 0.9 mL·min^-1. The wavelength of the detector was 240 nm. Results The linear ranges of aconitine in the heart, spleen, lung and kidney were 0.4-100 μg·mL^-1, the correlation coefficients were 0.997 2, 0.998 6, 0.999 3 and 0.999 4, respectively. The linear range of aconitine in liver was 2-200 μg·mL^-1 and the correlation coefficient was 0.999 0. The linear ranges of hypaconitine in heart, liver, spleen, lung, kidney, brain and spinal cord were 5-100 μg·mL^-1, the correlation coefficients were 0.999 4, 0.999 7, 0.999 8, 0.998 4, 0.999 8, 0.999 8 and 0.999 7, respectively. Detection limits (S/N=3) of aconitine and hypaconitine were 0.4 μg·mL^-1. The recoveries of aconitine and hypaconitine ranged from 88.7% to 102.2% and 86.5% to 101.3%, respectively, and the RSD of precision of aconitine and hypaconitine was 10%. Conclusion It appears to be an accurate and effective method that can offer reference basis for in toxication of Radix aconiti preparata clinically.
出处
《药学学报》
CAS
CSCD
北大核心
2005年第6期539-543,共5页
Acta Pharmaceutica Sinica
基金
SupportedbytheMinistryofScienceandTechnologyofthePeople’sRepublicofChina.
关键词
制川乌
乌头碱
次乌头碱
组织分布
HPLC
Radix aconiti preparata
aconitine
hypaconitine
tissure distribution
HPLC