高效液相色谱法测定乐山栀子熊果酸含量

Determination of the Content of Ursolic Acid in Fructus Gardeniae by HPLC from Leshan City

目的为控制乐山栀子的质量,建立高效液相色谱法测定乐山栀子中熊果酸含量的方法。方法采用高效液相色谱法,以熊果酸为化学对照品,固定相：UltimateTMC18键合硅胶柱（4.6 mm×250 mm,5μm）,流动相：甲醇∶水∶冰醋酸∶三乙胺（90∶10∶0.03∶0.06）,流速0.6 ml·min^-1,温度25℃,波长210 nm测定乐山栀子熊果酸含量。结果熊果酸在0.1-3.0μg范围内峰面积A与其质量M呈现良好的线性关系,其回归方程为：A=-12 954.882 9＋452 850.960 3M,r=0.999 6,n=7;3批乐山栀子中熊果酸的含量分别为（0.255 5±0.001 6）mg·g^-1药材,RSD=0.622 1%,n=4;（0.265 825±0.003 491）mg·g^-1药材,RSD=1.313%,n=4;（0.258 875±0.006 198）mg·g^-1药材,RSD=2.394%,n=4;精密度实验RSD=1.754%,仪器精密度良好;稳定性实验RSD=3.493%,在3.5 h测定熊果酸的含量是稳定的;重现性实验RSD=0.905 1%,平均回收率101.9%。结论高效液相色谱法适合乐山栀子中熊果酸的含量测定,该方法操作简便,结果稳定,精密度、重现性、回收率较好,值得推广。

Objective To establish the method of determining the cotent of ursolic acid in Fructus Gardeniae by HPLC. Methotis HPLC was used to determine the content of Ursolic acid in Fructus Gardenice ursolic acid as the standard, Solid phase.. UltimateTM C18（4.6 mm ×250 mm,5 μm）, Liquid phase： Methyiaicohol： Water： Acetic acid： Triethylaminum （90： 10：0.03 ： 0.06）, Flow rate： 0.6ml· min^ -1, temperature： 25℃, wavelength ： 210 nm. Results The calibration curve was linear in the range of 0.1 - 3.0μg, and the return formula was A = - 12954.882 9 ＋ 452 850.960 3 M, r = 0. 999 6, n = 7, the contents of ursolic acid in Frctus Cardeniae were （0.255 5 ±0.0016）mg ·g^-1 ,RSD=0.622 1% ,n =4;（0.265 825 ＋0.003 491 ）mg ·g^-1, RSD = 1. 313% ,n =4; （0. 258 875 ＋0. 006 198） mg ·g^-1 ,RSD =2. 394% ,n =4, respectively. Precision RSD = 1. 754% ,stablity RSD% =3.493,repeatability RSD =0.9051% ,recovery rate was 101.9%. Conelusion HPLC is suitable for the determination of ursolic acid in Fructus Gardeniae from Leshan city. This method is simple, the result is stable and has good repeatability, recovery and precision. It can be widely used for the quality control of Fructus Gardeniae.