山茱萸不同炮制品中8个化学成分的含量测定

Determination of Eight Major Components in Different Processed Products of Corni Fructus

目的:建立高效液相色谱法(HPLC)测定不同方法炮制的山茱萸中没食子酸、5-羟甲基糠醛、莫诺苷、獐牙菜苷、马钱苷、山茱萸新苷Ⅰ、齐墩果酸和熊果酸的含量,阐述不同炮制方法对山茱萸中8个成分含量的影响。方法:采用HPLC,色谱柱为StamsilC_(18)(250 mm×4.6 mm,5μm),流动相为乙腈-0.1%磷酸水溶液,梯度洗脱,流速为1.0 mL·min^(-1),检测波长分别为218、284、240、360 nm,柱温为30℃。结果:没食子酸、5-羟甲基糠醛、莫诺苷、獐牙菜苷、马钱苷、山茱萸新苷Ⅰ、齐墩果酸、熊果酸线性范围分别为0.80~32.07(r=0.9994)、0.02~0.73(r=0.9995)、26.91~1076.27(r=0.9994)、0.51~20.47(r=0.9991)、12.47~498.80(r=0.9997)、4.29~171.60(r=0.9996)、6.59~263.67(r=0.9995)、2.87~114.87μg·mL^(-1)(r=0.9991);精密度、稳定性、重复性试验RSD均小于3.0%;平均加样回收率为99.48%~104.32%(n=9),RSD均小于3.0%。与生品相比,山茱萸经炮制后熊果酸、没食子酸、齐墩果酸、5-羟甲基糠醛含量增加,马钱苷、莫诺苷、獐牙菜苷、山茱萸新苷Ⅰ含量减少。结论:该方法操作重复性好、准确、简便,可同时测定山茱萸不同炮制品中8个化学成分的含量。

Objective:To establish a high performance liquid chromatography(HPLC)method for the content determination of gallic acid,5-hydroxymethyl-2-furaldehyde,morroniside,sweroside,loganin,cornuside I,oleanolic acid,and ursolic acid in different processed products of Corni Fructus,and expound the effects of different processing methods on eight components in Corni Fructus.Methods:The HPLC analysis was performed on a Stamsil C_(18)(250 mm×4.6 mm,5μm)column.The mobile phase was a mixture of acetonitrile and 0.1%phosphoric acid for gradient elution.The flow rate and column temperature were set at 1.0 mL·min^(-1) and 30℃,respectively.The detection was conducted at the wavelengths of 218,284,240,360 nm.Results:The linear ranges for gallic acid,5-hydroxymethyl-2-furaldehyde,morroniside,sweroside,loganin,cornuside I,oleanolic acid,and ursolic acid were 0.80-32.07(r=0.9994),0.02-0.73(r=0.9995),26.91-1076.27(r=0.9994),0.51-20.47(r=0.9991),12.47-498.80(r=0.9997),4.29-171.60(r=0.9996),6.59-263.67(r=0.9995),2.87-114.87μg·mL^(-1)(r=0.9991),respectively.The RSD values of precision,stability,and reproducibility tests were all lower than 3.0%.The average recovery rates were within the range of 99.48%-104.32%(n=9),with the RSDs less than 3.0%.Compared with the raw Corni Fructus,the processed ones exhibited increased ursolic acid,gallic acid,oleanolic acid,and 5-hydroxymethyl-2-furaldehyde but decreased loganin,morroniside,sweroside and cornuside I.Conclusion:The method is reproducible,accurate,and simple,which can be used for simultaneously determining the contents of eight chemical components in different processed products of Corni Fructus.