Li Wen-Dong, Ma Chen
Institute of Materia Medica, Chinese Academy of Medical Sciences and Peking Union Medical College, Beijing 100050, China.
Yao Xue Xue Bao. 2005 Jun;40(6):539-43.
To develop an HPLC method for the determination of Aconitum alkaloids extracted from Radix aconiti preparata in rats.
Waters 2690@996 PAD system was used. The analytical column was a Halsil 100 C18 column (250 mm x 4.6 mm ID, 5 microm). 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.
The linear ranges of aconitine in the heart, spleen, lung and kidney were 0.4-100 microg.mL(-1), the correlation coefficients were 0.9972, 0.9986, 0.9993 and 0.9994, respectively. The linear range of aconitine in liver was 2-200 microg.mL(-1) and the correlation coefficient was 0.9990. The linear ranges of hypaconitine in heart, liver, spleen, lung, kidney, brain and spinal cord were 5-100 microg.mL(-1), the correlation coefficients were 0.9994, 0.9997, 0.9998, 0.9984, 0.9998, 0.9998 and 0.9997, respectively. Detection limits (S/N = 3) of aconitine and hypaconitine were 0.4 microg.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%.
It appears to be an accurate and effective method that can offer reference basis for in toxication of Radix aconiti preparata clinically.
建立一种用于测定大鼠制川乌提取物中乌头生物碱的高效液相色谱法。
采用Waters 2690@996 PAD系统。分析柱为Halsil 100 C18柱(250 mm×4.6 mm内径,5微米)。流动相为水、甲醇和二乙胺,比例为75:25:0.1。流速为0.9 mL·min⁻¹。检测器波长为240 nm。
乌头碱在心脏、脾脏、肺和肾脏中的线性范围为0.4 - 100微克·mL⁻¹,相关系数分别为0.9972、0.9986、0.9993和0.9994。乌头碱在肝脏中的线性范围为2 - 200微克·mL⁻¹,相关系数为0.9990。次乌头碱在心脏、肝脏、脾脏、肺、肾脏、脑和脊髓中的线性范围为5 - 100微克·mL⁻¹,相关系数分别为0.9994、0.9997、0.9998、0.9984、0.9998、0.9998和0.9997。乌头碱和次乌头碱的检测限(信噪比 = 3)为0.4微克·mL⁻¹。乌头碱和次乌头碱的回收率分别为88.7%至102.2%和86.5%至101.3%,乌头碱和次乌头碱精密度的相对标准偏差为10%。
这似乎是一种准确有效的方法,可为临床制川乌中毒提供参考依据。