高效液相色谱法测定川芎内酯软胶囊中4种苯酞成分

Simultaneous determination of 4 phthalidesins in Chuanxiong phthalide soft capsules by HPLC

目的建立高效液相色谱法同时测定川芎内酯软胶囊中苯酞类化学成分洋川芎内酯-Ⅰ、洋川芎内酯-H、瑟丹酸内酯、藁本内酯的含量。方法 Shiseido Capcell Pak C18 MGⅡ色谱柱（4.6 mm×150 mm,5μm）,流动相：甲醇-0.5%冰醋酸溶液,梯度洗脱,流速：0.7 m L·min^-1,柱温：30℃,检测波长为280 nm,进样量：10μL。结果 4个化合物与周围干扰峰达到基线分离,线性范围分别为洋川芎内酯-Ⅰ0.193 3-4.832μg·mL^-1（r=0.993 8）;洋川芎内酯-H 0.080 64-2.016μg·mL^-1（r=0.999 8）;瑟丹酸内酯3.415-85.38μg·mL^-1（r=0.999 8）;藁本内酯11.79-294.7μg·mL^-1（r=0.999 2）。RSD均〈2%（n=6）,平均加样回收率在95%-102%（n=6）。川芎内酯软胶囊中洋川芎内酯-Ⅰ、洋川芎内酯-H、瑟丹酸内酯、藁本内酯的含量分别为0.335 0、0.112 0、6.208、16.84 mg·g^-1（n=3）。结论该法简便、快捷、结果准确、重复性好、实用性强,可用于川芎内酯软胶囊的质量控制。

Objective To establish a HPLC-UV method to determine the content of senkyunolide Ⅰ, senkyunolide H, sedanenolide, and ligustilidein in Chuanxiong phthalide soft capsules. Methods Shiseido Capcell Pak C18 MG Ⅱ（150 mm×4.6 mm,5 μm） column was used. The mobile phase was consisted of methanol（A） and 0.5%（v/v） acetic acid solution（B） with gradient elution. The flow rate was 0.7 m L·min^-1, the column temperature was 30 ℃, the detection wavelength was 280 nm, and the injection volume was 10 μL. Results The 4 compounds and the unknown were separated with baseline. The linearity was 0.193 3-4.832 μg·mL^-1（r = 0.993 8） for senkyunolide Ⅰ, 0.080 64-2.016 μg·mL^-1（r = 0.999 8） for senkyunolide H, 3.415- 85.38 μg·mL^-1（r = 0.999 8） for sedanenolide, and 11.79-294.7 μg·mL^-1（r = 0.999 2） for ligustilide. The precision was within 2%（n = 6）, and the average recovery was at 95%- 102%（n = 6）. The content of senkyunolide Ⅰ, senkyunolide H, sedanenolide, and ligustilide in Chuanxiong phthalide soft capsules were 0.335 0, 0.112 0, 6.208, and 16.84 mg·g^-1（n = 3）, respectively. Conclusion The method is rapid, convenient, accurate, robust and suitable for the quality control of Chuanxiong phthalide soft capsules.