目的 建立头风痛丸中氧化前胡素、欧前胡素、异欧前胡素、洋川芎内酯H、洋川芎内酯I、洋川芎内酯A、瑟丹酸内酯、藁本内酯的HPLC法测定方法及其化学计量学综合质量评价方法。方法 使用Waters Symmetryshield C₁₈柱（250 mm×4.6 mm，5 μm），以甲醇-0.1%冰醋酸溶液为流动相，梯度洗脱，检测波长分别为310 nm（0~22 min检测氧化前胡素、欧前胡素和异欧前胡素）、280 nm（22~60 min检测川洋川芎内酯H、洋川芎内酯I、洋川芎内酯A、瑟丹酸内酯、藁本内酯），柱温30℃，体积流量1.0 mL/min，进样量10 μL。采用统计软件对头风痛丸中8种成分的含量数据进行主成分分析与聚类分析。结果 8种成分的线性范围分别为14.27~356.75、10.85~271.25、4.09~102.25、0.58~14.50、0.96~24.00、2.54~63.50、1.22~30.50、4.89~122.25 μg/mL（r ≥ 0.999 2）；平均加样回收率分别为100.05%、99.50%、99.38%、97.32%、96.98%、97.78%、96.93%、98.91%，RSD值分别为0.66%、0.59%、1.13%、0.99%、1.22%、1.07%、1.41%和0.78%（n=9）。15批样品提取出3个主成分，聚类分析分成2类。结论 以氧化前胡素、欧前胡素、异欧前胡素、洋川芎内酯H、洋川芎内酯I、洋川芎内酯A、瑟丹酸内酯、藁本内酯同步测定的HPLC法可用于头风痛丸多指标质量评价。

Objective To establish a method for the determination of oxypeucedanin, imperatorin, isoimperatorin, senkyunolide H, senkyunolide I, senkyunolide A, sedanolide, and ligustilide in Toufengtong Pills by HPLC and its chemometrics quality evaluation. Methods The separation and detection was performed on a Waters Symmetryshield C₁₈ (250 mm×4.6 mm, 5 μm) with linear gradient elution of methanol-0.1% aqueous acetic acid. The detection wavelengths were set at 310 nm (0-22 min for oxypeucedanin, imperatorin, and isoimperatorin) and 280 nm (22-60 min for senkyunolide H, senkyunolide I, senkyunolide A, sedanolide, and ligustilide). The column temperature was 30℃, the flow rate was set at 1.0 mL/min, and the injection volume was 10 μL. The principal component analysis and cluster analysis were conducted for the content results of eight constituents in Toufengtong Pills by statistical software. Results The linear ranges of eight components were 14.27-356.75, 10.85-271.25, 4.09-102.25, 0.58-14.50, 0.96-24.00, 2.54-63.50, 1.22-30.50, 4.89-122.25 μg/mL(r ≥ 0.999 2), whose average recoveries were 100.05%, 99.50%, 99.38%, 97.32%, 96.98%, 97.78%, 96.93%, and 98.91% with the RSD values of 0.66%, 0.59%, 1.13%, 0.99%, 1.22%, 1.07%, 1.41%, and 0.78% (n=9), respectively. Three main components belonged to the samples of the 15 batches of samples, and the samples of 15 batches of Toufengtong Pills could be divided into 2 categories. Conclusion Simultaneous determination of oxypeucedanin, imperatorin, isoimperatorin, senkyunolide H, senkyunolide I, senkyunolide A, sedanolide, and ligustilide by HPLC can be used to evaluate the quality of Toufengtong Pills.

R286.02

河南省重大科技专项（创新示范专项）项目（191110311100）