HPLC法测定青川栀子熊果酸含量

DETERMINATION OF THE CONTENT OF URSOLIC ACID IN FRUCTUS GARDENIAE FROM QINGCHUAN DISTRICT BY HPLC

目的:为控制青川栀子的质量,建立高效液相色谱法测定青川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:UltimateTM C18键合硅胶柱(4.6mm×250mm,5μm),流动相:甲醇:水:冰醋酸:三乙胺(90∶10:0.03∶0.06),流速:0.6ml·min-1,温度:25℃,波长:210nm测定青川栀子熊果酸含量。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=-12954.8829+452850.9603M,γ=0.9996,n=7;三批青川栀子中熊果酸的含量分别为(0.257±0.003866)mg·g-1,RSD=1.501%,n=4;(0.271±0.000758836)mg·g-1,RSD=0.281,n=4;(0.274±0.00372424)mg·g-1,RSD=1.357,n=4;精密度试验RSD%=1.754,仪器精密度良好;稳定性试验RSD%=3.493,在3.5h测定熊果酸的含量是稳定的;重现性试验RSD%=0.9051、平均回收率101.9%。结论:高效液相色谱法适合青川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.Methods：HPLC was used to determine the content of Ursolic acid in Fructus Gardenice,With Ursolic acid as the reference,Solid phase： UltimateTM C18（4.6mm×250mm,5μm）, Liquid phase： MethyiaicohohWater：Aeetic acid：Triethylaminum （90：10：0.03：0.06） ,Flow rate：0.6ml, min^-1, temperature：25℃ ,wavelength：210nm.Results： The calibration curve is very good linear in the range of 0.1-3.0μg,and the regression formula is A=-12954.8829＋ 452850.9603M （r=-0.9996）, the contents of Ursolic acid in Fructus Gardeni were （0.257±0.003866）mg·g^-1, RSD= 1.501%, n =4; （0.271 ±0.000758836）mg·g^-1, RSD =0.281, n =4; （0.274 ±0.00372424）mg·g^-1, RSD =1.357, n =4; respectively, precision is RSD% =1.754;stablity RSD% =3.493;repeatability RSD% =0.9051;recovery 101.9%. Conclusion： HPLC is suitable for the determination of Ursolic acid in Fructus Gardeniae from Qingchuan county. This method operated convenientely,the result is stable and has good repeatability,recovery and precision.It can be widely used for the quality control of Fructus Gardeniae.