中药橘核质量标准研究

Study on quality standard of Chinese medicine tangerine seed

目的建立中药橘核中柠檬苦素、诺米林、黄柏酮高效液相色谱含量测定方法。方法采用高效液相色谱法,色谱柱:Agilent SB-C 18(4.5 mm×250 mm,5μm),流动相乙腈-水(64∶36)等度洗脱,柱温:30℃,检测波长:210 nm,流速:1.0 mL·min^-1,进样量:10μL。结果柠檬苦素、诺米林、黄柏酮分别在0.396~3.960、0.404~4.040、0.392~3.920μg;柠檬苦素、诺米林、黄柏酮定量限分别为1.07、1.34、1.48 ng;检测限分别为0.39、0.22、0.35 ng。柠檬苦素平均加样回收率为100.23%,RSD为0.21%;诺米林平均加样回收率为99.89%,RSD为0.89%;黄柏酮平均加样回收率为100.68%,RSD为1.13%。结论本研究开发的中药橘核中柠檬苦素、诺米林、黄柏酮高效液相色谱含量测定方法,操作简便,重复性高,稳定性、精密性良好,可用于橘核的质量控制。

Objective To establish an HPLC method for the determination of limonin,nomilin and obacunone in the tangerine seed of traditional Chinese medicine.Methods The column:Agilent SB-C 18(4.5 mm×250 mm,5μm),the mobile phase acetonitrile-water(64∶36)isocratic elution,the column temperature:30℃,the detection wavelength:210 nm,the flow rate:1.0 mL·min^-1,the injection amount:10μL.Results The quantitative limits of limonin,nomilin and obacunone were 0.396~3.960,0.404~4.040 and 0.392~3.920μg,respectively;The quantitative limits of limonin,nomilin and obacunone were 1.07,1.34 and 1.48 ng,and the detection limits were 0.39,0.22 and 0.35 ng,respectively.The average recovery of limonin was 100.23%,RSD was 0.21%,the average recovery of nomilin was 99.89%,RSD was 0.89%,and the average recovery of obacunone was 100.68%,RSD was 1.13%.Conclusion The method for determination of limonin,nomilin and obacunone in the orange nucleus developed by this research was simple,reproducible,stable and precise.It can be used for the quality control of tangerine seed.