川乌和制川乌中单酯及双酯型生物碱成分的含量测定  

HPLC Determination of Aconitum Alkaloids and Their Hydrolysis Products in Radix Aconiti and Its Preparata

作　　者：张聿梅[1] 鲁静[1] 蒋渝 杨鲲[3] 李亚荣[4] 程显隆[1] 何轶[1] 林瑞超[1] 

机构地区：[1]中国药品生物制品检定所,北京100050 [2]永州市药品检验所,永州425000 [3]淮安市药品检验所,淮安223200 [4]吉林市药品检验所,吉林132011

出　　处：《药物分析杂志》2005年第7期807-812,共6页Chinese Journal of Pharmaceutical Analysis

基　　金：北京市科学技术委员会资助课题(H010210630111)

摘　　要：目的:建立川乌和制川乌中单酯及双酯型生物碱成分的高效液相色谱含量测定方法。方法:采用DiamonsilTM C18 5μm, 4.6 mm×250 mm色谱柱,流动相A[乙腈-四氢呋喃(25:15)]-流动相B[0.1 mol·L-1醋酸铵(1000 mL含冰醋酸 0.5 mL)]梯度洗脱,流速:0.8 mL·min-1,检测波长:235 nm。结果:乌头碱、次乌头碱、新乌头碱、苯甲酰新乌头碱和苯甲酰次乌头碱分离良好,各成分浓度与HPLC峰面积呈良好的线性关系,线性范围分别是:乌头碱0.01-0.36(r=0.9996),0.32 -5.16μg(r=0.9999);次乌头碱0.01-1.06(r=0.9999),0.05-1.32 μg(r=0.9999),1.29-20.60μg(r=0.9999);新乌头碱0.22-3.59μg(r=0.9999);苯甲酰新乌头碱0.02-0.10(r=0.9997),0.13-2.04μg(r=0.9998);苯甲酰次乌头碱 0.02-0.12(r=0.9996),0.15-2.41μg(r=0.9999)。平均回收率分别为105.0%(RSD=4.4%),104.9%(RSD=1.8%), 100.4%(RSD=3.0%);107.6%(RSD=3.3%),104.2%(RSD=1.5%),102.9%(RSD=1.9%);112.2%(RSD=3.2%), 106.3%(RSD=1.5%),103.5%(RSD=2.3%);104.1%(RSD=2.2%);100.8%(RSD=2.9%)。结论:建立的HPLC法专属,准确,耐用性良好。采用本法测定了23批不同产地及不同炮制方法得到的川乌和制川乌药材中新乌头碱、次乌头碱、乌头碱、苯甲酰新乌头碱和苯甲酰次乌头碱的含量,为川乌及饮片质量标准的建立提供了依据。Objective:To establish an HPLC method for determination of five alkaloids (aconitine,hypaconitine, mesaconitine and their hydrolysis products, benzoylmesaconine and benzoylhypaconine).Method:The separation was performed on a Diamonsil?C18 analysis column,the mobile phase consisted of acetonitrile-tetrahydrofuran(25:15, phase A) ,0.1 mol·L-1 ammonium acetate (per 1000 mL contains 0. 5 mL acetic acid, phase B ) with gradient elu-tion with flow rate of 0.8 mL·min-1, and detector at 235 nm. Results: The calibration curves were linear in the range of 0.01-0.36μg (r =0.99%) ,0.32-5.16 μg(r=0.9999) for aconitine,0.01-1.06μg (r=0.9999), 0.05-1.32μg (r=0.9999), 1.29-20.60μg (r=0.9999) for hypaconitine,0.22-3.59μg(r=0.9999) for mesaconitine,0.02-0.10μg(r=0.9997),0.13-2.04μg(r=0.9998) for benzoylmesaconine,and 0.02-0.12μg (r=0.9996) ,0.15-2.41μg (r=0.9999) for benzoylhypaconine. The average recoveries were 105.0% (RSD= 4.4%), 104.9%(RSD=1.8%),100.4%(RSD=3.0%);107.6%(RSD=3.3% ),104.2% (RSD=1.5%), 102.9%(RSD=1.9%);112.2%(RSD=3.2%),106.3%(RSD=1.5%),103.5% (RSD=2.3%);104.1%(RSD =2.2%);100.8%(RSD=2.9% )respectively.Conclusion:This method is accurate,and suitable for the determination of aconitum alkaloids and their hydrolysis products in Radix Aconiti,and its preparations. The method established in this paper can be adopted for the quality control of both Radix Aconiti,and the preparations.

关 键 词：生物碱成分 制川乌 次乌头碱 新乌头碱 含量测定方法 高效液相色谱 饮片质量标准 苯甲酰 平均回收率 HPLC法 梯度洗脱 四氢呋喃 检测波长 线性关系 线性范围 0.05 炮制方法 不同产地 流动相 色谱柱 冰醋酸 醋酸铵 峰面积 

分 类 号：R284.1[医药卫生—中药学] R291.2[医药卫生—中医学]