反相高效液相色谱法同时测定川芎中的四种内酯类化合物

Determination of Lactone Components in Chuanxiong by Reversed-Phase High Performance Liquid Chromatography

用反相高效液相色谱法同时测定了川芎中的4种主要内酯类成分(洋川芎内酯-H、洋川芎内酯-I、瑟丹酸内酯和蒿本内酯).采用XDB-C8柱,以甲醇-1%乙酸水溶液为流动相进行梯度洗脱,甲醇-1%乙酸水溶液的体积比在15 min内从55:45线性变化至100:0,流速0.8 mL/min,紫外检测波长280 nm.4种内酯类化合物的检测限为0.011～0.027 μg,回收率为96% ～108% .该方法操作简单,结果准确,重现性好,可用于川芎药材及饮片中4种内酯类化合物的同时测定,具有很高的实用价值.

A reversed-phase high performance liquid chromatographic method was developed for the simultaneous determination of four main lactone components including senkyunolide-H, senkyunolide-Ⅰ, sedanenolide and Z-ligustilide in Chuanxiong, a Chinese herbal medicine. The samples were pretreated using ultrasonic extraction, and 80% ethanol was used as extractant in the experiment. The chromatographic analysis was carried out using an XDB-Cs column and the mobile phase consisted of methanol-1% （volume fraction） acetic acid water （55：45→,100： 0, v/v, in 15 min）. The flow rate was 0.8 mL/min. A diode array detector was used to detect the compositions and 280 nm was chosen as the detection wavelength. The whole process could be performed within 15 min. The operating curves were found to be linear over the ranges of 0.4 - 2.2 mg/L （r=0.9992）,0.4-2.2mg/L （r=0.9979）, 2.6-7.8mg/L （r=0.9992） and 4.8- 14.3 mg/L （r = 0. 999 8 ） and the detection limits （S/N = 3 ） were 0. 024, 0. 027, 0. 018 and 0.011 p.g for senkyunolide-H, senkyunolide-Ⅰ, sedanenolide and Z-ligustilide, respectively. The recoveries of the four lactone components were found in the range of 96% - 108%. The rapid and accurate method has been successfully applied to the simultaneous determination of the four lactone components in Chuanxiong.