UPLC同时测定伤科跌打片中6种有效成分的含量

Simultaneous determination of six components in Shangke Dieda Tablets by UPLC

目的:建立伤科跌打片中芍药苷、柚皮苷、橙皮苷、新橙皮苷、木香烃内酯、去氢木香烃内酯的UPLC测定方法。方法:色谱柱为Agilent Poroshell 120 SB-C_(18) 100 mm×4.6 mm, 2.7μm),采用二元梯度洗脱,流动相A为乙腈,B为0.1%磷酸水溶液,柱温为30℃,流速1.0 mL·min^(-1),检测波长为230 nm。结果:芍药苷、柚皮苷、橙皮苷、新橙皮苷、木香烃内酯、去氢木香内酯6种成分在考察的进样量范围内,进样浓度与峰面积之间呈良好的线性关系(r﹥0.999),线性范围分别为0.854 2~256.272μg·mL^(-1)(r=0.999 9)、1.057 5~317.247μg·mL^(-1)(r=0.999 9)、0.989 5~269.850μg·mL^(-1)(r=0.999 9)、1.055 6~316.689μg·mL^(-1)(r=0.999 9)、0.9051~271.527μg·mL^(-1)(r=0.999 8)、1.064 7~319.395μg·mL^(-1)(r=0.999 9);平均加样回收率分别为99.4%(RSD=1.2%),104.0%(RSD=1.2%),101.6%(RSD=1.0%),102.9%(RSD=0.4%),97.0%(RSD=1.9%),104.2%(RSD=1.0%)。收集10个生产企业共74批样品,测得样品含量分别为芍药苷0.250 8~0.653 2 mg/片,柚皮苷0.042 2~0.930 9 mg/片,橙皮苷0.590 9~3.978 0 mg/片、新橙皮苷0.021 2~0.592 6 mg/片、木香烃内酯0.002 4~0.156 7 mg/片、去氢木香内酯0.009 2~0.231 3 mg/片。结论:本法经方法学验证,可用于伤科跌打片的质量控制。

Objective:To establish a UPLC method for the simultaneous determination of paeoniflorin,naringin,hesperidin,neohesperidin,costunolide and dehydrocostuslactone to improve the quality standard of Shangke Dieda Tablets.Methods:An Agilent Poroshell 120 C 18 column(100 mm×4.6 mm;2.7μm)was used with a mobile phase of acetonitrile and 0.1%phosphate solution with binary gradient system at a flow rate of 1.0 mL·min-1.The detection wavelength was 230 nm and the column temperature was 30℃.Results:Paeoniflorin,naringin,hesperidin,neohesperidin,cosinolide and dehydrocosinolide showed a good linear relationship between injection concentration and peak area(r>0.999).The linear ranges of six components were 0.8542-256.272μg·mL^(-1)(r=0.9999),1.0575-317.247μg·mL^(-1)(r=0.9999),and 0.9895-269.850μg·mL^(-1)(r=0.9999),1.0556-316.689μg·mL^(-1)(r=0.9999),0.9051-271.527μg·mL^(-1)(r=0.9998),and 1.0647-319.395μg·mL^(-1)(r=0.9999),respectively.The average recoveries of six components were 99.4%(RSD=1.2%),104.0%(RSD=1.2%),101.6%(RSD=1.0%),102.9%(RSD=0.4%),97.0%(RSD=1.9%),and 104.2%(RSD=1.0%),respectively.A total of 74 batches of samples were collected from 10 manufacturers.The contents of paeoniflorin,naringin,hesperidin,neohesperidin,coxinolactone,and dehydrocosinolactone were 0.2508-0.6532,0.0422-0.9309,0.5909-3.9780,0.0212-0.5926,0.0024-0.1567,0.0092-0.2313 mg per tablet,respectively.Conclusion:The validated results showed that the method can be used to control the quality of Shangke Dieda Tablets.