高效液相色谱法测定丹芩滴丸中黄芩苷和隐丹参酮含量

Determination of baicalin and cryptotanshinone in Danqin dropping pills by HPLC

目的:建立丹芩滴丸中黄芩苷和隐丹参酮含量测定方法。方法:采用高效液相色谱法。IntersilC18分析色谱柱(4.6mm×250mm,5μm),流动相A为85%乙腈(含0.5%三乙胺,磷酸调pH3.0),流动相B为10%乙腈(含0.5%三乙胺,磷酸调pH3.0)。梯度洗脱程序:0～15min,A20%～100%,B80%～0%;流速:1.0mL·min-1,检测波长:270nm。结果:黄芩苷和隐丹参酮保留时间分别为6.7min和19.3min,黄芩苷回归方程Y=1100430+81892541X,r=0.9999,线性范围0.2402～1.201μg;隐丹参酮回归方程Y=695415+147227894X,r=0.9999,线性范围0.1600～0.8000μg。黄芩苷和隐丹参酮最低检出量分别为0.0051μg和0.0045μg。黄芩苷平均回收率为97.4%,RSD为2.4%,隐丹参酮平均回收率为97.3%,RSD为2.1%。结论:本方法操作简便,结果准确可靠,可用于丹芩滴丸中黄芩苷和隐丹参酮的含量测定。

OBJECTIVE To develop a HPLC quantitative method for simultaneous determination of Baicalin and Cryptotanshinone in Danqin dropping pills. METHODS The chromatographic conditions include column Intersil C18 ,mobile phase A： 85% acetonitrile containing 0. 5 % triethylamine was adjusted to pH 3. 0 by phosphoric acid, mobile phase B： 10 % acetonitrile containing 0. 5% triethylamine was adjusted to pH 3. 0 by phosphoric acid with gradient eluation. The gradient eluation program： 0 - 15 min, A 20% -100%, B 80% - 0% with a flow rate of 1 mL·min^-1 and monitored at 270 nm RESULTS The retention times of baicalin and cryptotanshinone were 6. 7 min and 19. 3 min separately. The number of theoretical plates caculated by baicalin and cryptotanshinone peaks were 3 600 and 7 500 respectively. The regression equation for baicalin was Y = 110 043 0 ＋ 818 925 41X , r = 0. 999 9, and the linear range was 0. 2402- 1. 201μg; The regression equation for cryptotanshinone was Y= 695 415＋ 147 227 894X ,r = 0. 999 9 and thelinear range was 0. 160 0 - 0. 800 0μg. The average recoveries of baicalin and cryptotanshinone were 97. 4%, （RSD 2.4% ） and 97. 3% , （RSD 2.1%） separately. The measurable lowest limit （S/N = 3） of baicalin and cryptotanshinone were 0. 0051 μg and0. 0045μg respectively. CONCLUSION The method is sensitive,rapid and accurate for the determination of baicalin and cryptotanshinone in Danqin dropping pills.