椒莪合剂的质量标准研究

Studies on the Quality Standard of Jiao'e Mixture

目的：检测椒莪合剂中主要化学成分含量并制订其质量标准。方法：1采用TLC法对制剂中莪术醇、牻牛儿酮、莪术二酮及α-亚麻酸进行鉴别;2采用HPLC法,以Intersustain C18色谱柱（4.6 mm×250 mm,5.0μm）,检测波长为216 nm,以乙腈-水作为流动相运用梯度洗脱法分别测定制剂中牻牛儿酮、呋喃二烯的含量;以乙腈-1%醋酸溶液（90：10）为流动相,Kromasil C18色谱柱（4.6 mm×200 mm,5.0μm）,检测波长为205 nm,测定制剂中α-亚麻酸的含量。结果：1制剂中牻牛儿酮、莪术二酮及α-亚麻酸的薄层鉴别具有较好的专属性;2牻牛儿酮、呋喃二烯及α-亚麻酸的线性范围与相关系数（r）分别为0.0060~0.1200 mg·m L-1、0.9995,0.0120~0.2400 mg·g-1、0.9995,6.90~115.00 mg·g-1、0.9998;3牻牛儿酮、呋喃二烯及α-亚麻酸平均加样回收率与RSD分别为98.65%、0.65%,99.02%、0.55%,98.49%、0.67%;43批制剂中牻牛儿酮、呋喃二烯及α-亚麻酸的平均含量（mg·g-1）分别为18.42、53.87和277.10 mg·g-1,RSD（%）分别为1.18、0.68和1.37%。结论：所建立的制剂中牻牛儿酮、呋喃二烯及α-亚麻酸检测方法科学、合理,可用于其质量控制。

Objective： To determine the content of main chemical components in Jiao＇e mixture and establish its quality standard. Methods： ①Curcumenol, Germacrone, Curdione and ct-linolenic acid in the preparation were identified by TLC, respectively. Germacrone and Furanodiene in the preparation were analyzed on Intersustain C18 （4.6 mm·250 mm, 5.0 μm） with acetonitrile-water as mobile phases＇in gradient elution manner, and the detection wavelength was set up at 216 nm. ②The quantative analysis of a-linolenic acid was carried out on a column of Kromasil C18 （4.6 mm×200mm, 5.0μm）, using a mobile phase of acetonitrile-water （containing 1% acetic acid）（90：10） at the wavelength of 205 nm. Results： ①The TLC of Germacrone, Curdione and a-linolenic acid in the preparation showed good specificity. ②The linear range and correlation coefficient of Germaerone, Furanodiene and a-linolenic acid were 0.0060-0.1200 mg·mL^-1, 0.9995, 0.0120-43.2400 mg·mL^-1, 0.9995 and 6.90-115.00 mg·mL^-1, 0.9998, respectively. ③The average recoveries and RSD ofGermaerone, Curdione and et-linolenic acid were 98.65 %, 0.65 %, 99.02 %, 0.55 % and 98.49 %, 0.67 %, respectively. ④The average contents （mg·mL^-1） of Germacrone, Curdione and a-linolenic acid were 18.42,53.87 and 277.10 mg·mL^-1, coupled with the average RSD （%） of 1.18, 0.68 and 1.37 % in the 3 batches of preparations. Conclusion： The determination method of Germacrone, Furanodiene and a-linolenic acid in the preparation is so scientific and reasonable that can be used for its quality control.