RP-HPLC同时测定活络效灵丹中糖苷及生物碱成分的含量

目的：建立反相高效液相色谱法同时测定活络效灵丹中3个糖苷（马钱苷酸、龙胆苦苷、芍药苷）和2个生物碱（延胡索乙素、延胡索甲素）成分的含量。方法：采用xBridge^Tm C₁₈色谱柱（150 mm×4.6 mm，3.5μm），流动相A为乙腈，流动相B为体积分数0.02%的磷酸水溶液，梯度洗脱，流速为1.2 mL·min^-1，检测波长为230 nm，柱温为30℃。结果：马钱苷酸、龙胆苦苷、芍药苷、延胡索乙素、延胡索甲素的质量浓度分别在9.375~300.0、45.99~1502.4、31.20~998.3、1.693~54.20、1.125~36.00 mg·L^-1范围内与峰面积呈良好的线性关系（r ≥ 0.9996，n=6），加样回收率均值分别为99.1%、99.9%、98.4%、102.2%、99.8%，RSD均不大于2.8%。3个糖苷和2个生物碱含量的质量分数测定结果分别为3.94~4.59、22.8~26.5、13.6~14.7、1.04~1.17、0.408~0.459 mg·g^-1。结论：该方法可作为活络效灵丹中糖苷和生物碱类化学成分的含量测定方法，为其质量控制提供参考依据。

Objective: To develop an RP-HPLC method for simultaneous determination of five constituents(loganic acid, gentiopicroside, paeoniflorin, tetrahydropalmatine, and corydaline)in Huoluo Xiaoling Dan. Methods: The analysis was carried out on an xBridge^Tm C₁₈ column(150 mm×4.6 mm, 3.5 μm). The mobile phase A was composed of acetonitrile and the mobile phase B 0. 02% phosphoric acid aqu. with gradient elution. The flow rate was 1.2 mL·min^-1, the detection wavelength was set at 230 nm, and the column temperature was 30℃. Results: The linear ranges of loganic acid, gentiopicroside, paeoniflorin, tetrahydropalmatine and corydaline were 9.375-300.0 mg·L^-1, 45.99-1 502.4 mg·L^-1, 31.20-998.3 mg·L^-1, 1.693-54.20 mg·L^-1, 1.125-36.00 mg·L^-1(r ≥ 0.999 6, n=6), respectively. The average recoveries of the five constituents were 99.1%, 99.9%, 98.4%, 102.2% and 99.8%, respectively with RSDs ≤ 2.8%. The contents of three glucosides and two alkaoids were in the range of 3.94-4.59 mg·g^-1, 22.8-26.5 mg·g^-1, 13.6-14.7 mg·g^-1, 1.04-1.17 mg·g^-1 and 0.408-0.459 mg·g^-1. Conclusions: The established method can be used for the determination of glucosides and alkaloids in Huoluo Xiaoling Dan, thus providing reference for quality control of Huoluo Xiaoling Dan.