高效液相色谱-蒸发光散射检测法测定鹤蟾片中贝母素甲和贝母素乙的含量

HPLC-ELSD determination of peimine and peiminine in Hechan tablets

目的:建立高效液相色谱-蒸发光散射检测法同时测定鹤蟾片中贝母素甲和贝母素乙的含量。方法:采用 HiQsil C_(18)(250 mm×4.6 mm,5 μm)色谱柱,柱温为25℃,以乙腈-甲醇-二乙胺(60:40:0.05)为流动相,流速为0.8 mL·min^(-1);蒸发光散射检测器检测,漂移管温度为80℃,气体流速为2.0 L·min^(-1)。结果:在选定的色谱条件下,以峰面积的常用对数(Y)对进样量的常用对数(X)进行线性回归,贝母甲素和贝母乙素的回归方程分别为 Y=1.557X+1.666和 Y=1.700X+1.571,线性范围分别为0.29～2.80μg(r=0.9996)和0.34～3.40μg(r=0.9999);加样回收率(n=5)分别为99.2%和99.4%,RSD 分别为2.7%和3.1%。结论:本法简便、准确,重复性好,可用于该制剂的质量控制分析。

Objective：To establish an HPLC - ELSD method for the determination of peimine and peiminine in Hechan tablets. Methods：Chromatography was performed on a HiQsil C 18 column （250 mm× 4. 6 mm ,5 μm）at 25 ℃. The mobile phase composition was acetonitrile- methanol- diethylamine（60： 40： 0. 05 ）with a flow rate of 0. 8 mL · min^-1. An evaporate light - scattering detector （ELSD） was used as detector with gas flow rate of 2. 0 L·min^-1 and drift tube temperature of 80 ℃. Results：The calibration curves of peimine and peiminine were linear in the ranges of 0. 29 - 2. 80 μg and 0. 34 - 3.40 μg, and their regressive equations were Y = 1. 557X ＋ 1. 666 （ r = 0. 9996 ） and Y = 1. 700X ＋ 1.571 （ r = 0. 9999 ） respectively. The average recoveries （ n = 5 ） of peimine and peiminine were 99.2% （RSD = 2. 7% ）, and 99. 4% （RSD = 3.1% ）, respectively. Conclusion：The method is reliable, simple, and accurate. It can be used to control this preparation.