UPLC波长切换法同时测定沉香化气丸中7个成分的含量

目的：建立UPLC波长切换法同时测定沉香化气丸中甘草苷、芸香柚皮苷、柚皮苷、橙皮苷、甘草酸、木香烃内酯和广藿香酮的含量。方法：采用Kinetex C₁₈色谱柱（4.6 mm×100 mm，2.7 μm），以乙腈（A）-0.1%磷酸水溶液（B）为流动相，梯度洗脱，流速0.8 mL·min^-1，波长切换（0~20 min，210 nm，检测甘草苷、芸香柚皮苷、柚皮苷、橙皮苷；20~25 min，254 nm，检测甘草酸；25~30.8 min，210 nm，检测木香烃内酯；30.8~34 min，310 nm，检测广藿香酮），柱温35 ℃。结果：待测成分峰与相邻峰达到基线分离，甘草苷、芸香柚皮苷、柚皮苷、橙皮苷、甘草酸、木香烃内酯和广藿香酮的质量浓度分别在1.659~39.82 μg·mL^-1（r=1.000）、1.729~41.50 μg·mL^-1（r=0.999 8）、0.663 4~15.93 μg·mL^-1（r=0.999 7）、9.637~240.9 μg·mL^-1（r=0.999 7）、2.127~51.06 μg·mL^-1（r=0.999 7）、1.794~43.08 μg·mL^-1（r=0.999 6）、0.9080~21.80 μg·mL^-1（r=0.999 4）范围内与峰面积呈良好的线性关系；平均加样回收率（n=6）分别为98.7%（RSD=2.4%）、101.7%（RSD=2.6%）、100.5%（RSD=2.9%）、99.0%（RSD=2.8%）、99.5%（RSD=2.5%）、99.3%（RSD=2.2%）、101.7%（RSD=1.7%）；方法重复性（n=6）的RSD均小于2.9%；供试品溶液在室温条件下24 h内稳定，RSD均小于1.8%。8批样品中甘草苷、芸香柚皮苷、柚皮苷、橙皮苷、甘草酸、木香烃内酯和广藿香酮7个成分的含量测定结果分别为0.424~0.989、0.482~0.802、0.105~0.204、3.170~4.842、0.702~0.997、0.183~0.916、0.216~0.385 mg·g^-1。结论：该方法为沉香化气丸的质量标准研究提供参考。

Objective:To develop a method for simultaneous determination the contents of liquiritin,narirutin,naringin,hesperidin,glycyrrhizic acid,costunolide and pogostone in Chenxiang Huaqi pills by UPLC with wavelength switching.Methods:The analyses were carried out on a Kinetex C₁₈ column(4.6 mm×100 mm, 2.7 μm)with the mobile phase consisting of acetonitrile and 0.1% phosphoric acid in a gradient mode at a flow rate of 1 mL·min^-1.The detection wavelength was set at 210 nm for liquiritin,narirutin,naringin and hesperidin in the first 20 min,254 nm for glycyrrhizic acid during 20-25 min,210 nm for costunolide during 25-30.8 min,310 nm for pogostone during 30.8-34 min.The column temperature was at 35℃.Results:Baseline separation of the analytes and their adjacent peaks reaching the standard by chromatography.Good linearity was obtained for liquiritin,narirutin,naringin,hesperidin,glycyrrhizic acid,costunolide and pogostone in ranges of 1.659-39.82 μg·mL^-1(r=1.000),1.729-41.50 μg·mL^-1(r=0.999 8),0.663 4-15.93 μg·mL^-1(r=0.999 7),9.637-240.9 μg·mL^-1(r=0.999 7),2.127-51.06 μg·mL^-1(r=0.999 7),1.794-43.08 μg·mL^-1(r=0.999 6),and 0.9080-21.80 μg·mL^-1(r=0.999 4),respectively.The average recoveries(n=6)of the above seven components were 98.7%(RSD=2.4%),101.7%(RSD=2.6%),100.5%(RSD=2.9%),99.0%(RSD=2.8%),99.5%(RSD=2.5%),99.3%(RSD=2.2%),and 101.7%(RSD=1.7%),respectively.The repeatability was good with RSD less than 2.9%.The seven analytes were stable at room temperature within 24 h with RSD less than 1.8%.The contents in 8 samples were in the ranges of 0.424-0.989 mg·g^-1 for liquiritin,0.482-0.802 mg·g^-1 for narirutin,0.105-0.204 mg·g^-1 for naringin,3.170-4.842 mg·g^-1 for hesperidin,0.702-0.997 mg·g^-1 for glycyrrhizic acid,0.183-0.916 mg·g^-1 for costunolide and 0.216-0.385 mg·g^-1 for pogostone.Conclusion:The method offered reference for quality standard of Chenxiang Huaqi pills.