枳实标准汤剂质量研究

Study on quality of Aurantii Fructus Immaturus standard decoction

为更好地评价不同产地的枳实标准汤剂,建立了枳实标准汤剂中辛弗林含量及特征图谱的测定方法。采用高效液相色谱仪与InertSustain AQ-C18(4.6 mm×250 mm,5.0μm)色谱柱,以甲醇-磷酸二氢钾溶液为流动相,柱温为28℃,流速为1.0 mL/min,检测波长为225 nm,对枳实标准汤剂中辛弗林含量、特征图谱进行了测定。结果显示,15批枳实标准汤剂出膏率均值为15.14%,范围为10.50%~19.91%,RSD为19.31%;辛弗林含量(质量分数)均值为9.07 mg/g,范围为5.92~15.21 mg/g,RSD为33.05%;辛弗林含量转移率均值为22.65%,范围为10.24%~47.70%,RSD为45.92%;15批枳实标准汤剂共确定7个共有峰,各峰相对保留时间均在±5%内,相对峰面积RSD均大于100%,相似度为0.655~0.936。这表明,不同产地的枳实出膏率、辛弗林含量及含量转移率较稳定;不同产地的枳实标准汤剂各成分间差异较大。经方法学考察认为,枳实标准汤剂中辛弗林含量及特征图谱的测定方法稳定,具有较高的重复性、稳定性及可信度,可用于枳实标准汤剂的质量评价,可为进一步深入研究枳实配方颗粒提供参考。

In order to better evaluate the standard decoction of Aurantii Fructus Immaturus from different producing areas,the determination method of synephrine content and characteristic spectrum in Aurantii Fructus Immaturus standard decoction was established.The method was performed on high performance liquid chromatography(HPLC)and InertSustain AQ-C18 column(4.6 mm×250 mm,5.0μm)with methanol-potassium dihydrogen phosphate solution as the mobile phase.The column temperature was 28℃,the flow rate was set at 1.0 mL/min and the detection wavelength was 225 nm,and then the synephrine content and characteristic spectrum in Aurantii Fructus Immaturus standard decoction was detected.The results show that the average extraction rate of 15 batches of Aurantii Fructus Immaturus standard decoction is 15.14%,it ranges from 10.50%to 19.91%,and RSD is 19.31%;The average synephrine content is 9.07 mg/g,it ranges from 5.92 to 15.21 mg/g,and RSD is 33.05%.The average content transfer rate of synephrine is 22.65%,it ranges from 10.24%to 47.70%,and RSD is 45.92%.There are 7 common peaks in 15 batches of Aurantii Fructus Immaturus standard decoction,the relative retention time of each peak is within±5%,the relative peak area RSD is greater than 100%,and the similarity is 0.655~0.936.In this study,the extraction rate,the content of synephrine and the content transfer rate of Aurantii Fructus Immaturus from different regions are relatively stable and there are significant differences among the ingredients in the standard decoction of Aurantii Fructus Immaturus from different regions.The methodology study shows that the method for the determination of synephrine and characteristic spectrum in Aurantii Fructus Immaturus standard decoction is stable,with high repeatability,stability and credibility.It can be used for the quality evaluation of Aurantii Fructus Immaturus standard decoction and provide reference for further study of Aurantii Fructus Immaturus formula particles.