摘要
目的 利用梯度洗脱 ,建立高效液相色谱测定丹参酮滴耳液中二氢丹参酮Ⅰ、隐丹参酮、丹参酮Ⅰ和丹参酮ⅡA 含量的方法。方法 采用高效液相色谱法。IntersilC18分析色谱柱 (4 6mm× 2 5 0mm ,5 μm) ,流动相为乙腈 10 %乙腈梯度洗脱 ,流速1 6mL·min-1,检测波长 2 5 4nm。结果 二氢丹参酮Ⅰ、隐丹参酮、丹参酮Ⅰ和丹参酮ⅡA 保留时间分别为 11 9,19 2 ,2 1 3和2 8 5min ,与各自相邻峰的分离度均大于 1 5 ,理论板数分别为 3310 ,4 2 78,36 2 4和 2 0 6 77。二氢丹参酮Ⅰ平均回收率为10 1 3% ,RSD =2 2 % ,隐丹参酮平均回收率为 97 2 % ,RSD =2 2 % ,丹参酮Ⅰ平均回收率为 10 2 1% ,RSD =3 0 % ,丹参酮ⅡA平均回收率为 99 5 % ,RSD =1 9%。二氢丹参酮Ⅰ、隐丹参酮、丹参酮Ⅰ和丹参酮ⅡA 最低检出浓度分别约为 0 6 ,0 9,0 6和0 3μg·mL-1。结论 本法操作简便 ,测定结果准确可靠 ,可用于丹参酮滴耳液中二氢丹参酮Ⅰ、隐丹参酮、丹参酮Ⅰ和丹参酮ⅡA 的含量测定。
OBJECTIVE A quantitative method was developed for the determination of dihydrotanshinone Ⅰ, cryptotanshinone, tanshinone Ⅰ and tanshinone Ⅱ A in tanshinone ear drops by HPLC. METHODS Column Intersil C 18 was used. The mobile phase was composed of acetonitrile - 10% acetonitrile with gradient eluation. The flow rate was 1.6 mL·min -1 with the wavelength at 254 nm. RESULTS The number of theoretical plates calculated by dihydrotanshinone Ⅰ, cryptotanshinone, tanshinoneⅠand tanshinoneⅡ A peak were 3?310, 4?278, 3?624 and 20?677 respectively. The average recoveries of dihydrotanshinone Ⅰ, cryptotanshinone, tanshinoneⅠ, tanshinone Ⅱ A were 101.3% (RSD=2.2%), 97.2% (RSD=2.2%), 102.1% (RSD=3.0%) and 99.5% (RSD=1.9%) respectively. The detection limits of dihydrotanshinone Ⅰ, cryptotanshinone, tanshinone Ⅰ and tanshinone Ⅱ A were about 0.6, 0.9, 0.6 and 0.3 μg·mL -1 respectively. CONCLUSION The method was sensitive, rapid and accurate.
出处
《中国药学杂志》
CAS
CSCD
北大核心
2004年第3期218-220,共3页
Chinese Pharmaceutical Journal