摘要
目的:建立HPLC波长切换法时测定心舒宁片中槲皮素、葛根素、山柰素、异鼠李素、毛冬青皂苷B2、毛冬青皂苷A1、毛冬青皂苷B1和冬青素A的含量。方法:采用Inertsil ODS-C18色谱柱(250 mm×4.6 mm,5μm),流动相为甲醇-0.4%磷酸溶液,梯度洗脱,流速为1.0 ml·min^-1,进样量为10μl,柱温为25℃,检测波长为360 nm(槲皮素、山柰素、异鼠李素)、250 nm(葛根素)、210 nm(毛冬青皂苷B2、毛冬青皂苷A1、毛冬青皂苷B1、冬青素A)。结果:槲皮素、葛根素、山柰素、异鼠李素、毛冬青皂苷B2、毛冬青皂苷A1、毛冬青皂苷B1和冬青素A的线性范围分别为10.406~208.120μg·ml^-1,15.426~308.520μg·ml^-1,2.358~47.160μg·ml^-1,5.352~107.040μg·ml^-1,2.688~53.760μg·ml^-1,6.620~132.400μg·ml^-1,5.784~115.680μg·ml^-1,21.604~432.080μg·ml^-1(r≥0.9994);平均加样回收率为98.4%~101.3%(RSD<2.0%,n=6);精密度、重复性、稳定性(24 h)试验的RSD<2.0%(n=6)。结论:所建立的方法稳定、可靠,可用于心舒宁片的质量控制。
Objective:To establish an HPLC with wavelength switching method for the simultaneous determination of quercetin,puerarin,kaempferol,isorhamnetin,ilexsaponin B2,ilexsaponin A1,ilexsaponin B1 and ilexgenin A in Xinshuning tablets.Methods:The determination was performed on an Inertsil ODS-C18 column(250 mm×4.6 mm,5μm)with the mobile phase consisting of methonal-0.4%phosphoric acid in a gradient mode.The flow rate was 1.0 ml·min^-1.The column temperature was set at 25℃and the injection volume was 10μl.The detection wavelength was set at 360 nm for ilexsaponin B2,ilexsaponin A1,ilexsaponin B1 and ilexgenin A,250 nm for kaempferol,and 210 nm for quercetin,kaempferol and isorhamnetin.Results:Quercetin,puerarin,kaempferol,isorhamnetin,ilexsaponin B2,ilexsaponin A1,ilexsaponin B1 and ilexgenin A showed good linear relationship within the range of 10.406-208.120μg·ml^-1,15.426-308.520μg·ml^-1,2.358-47.160μg·ml^-1,5.352-107.040μg·ml^-1,2.688-53.760μg·ml^-1,6.620-132.400μg·ml^-1,5.784-115.680μg·ml^-1 and 21.604-432.080μg·ml^-1(r≥0.9994),respectively.The average recoveries were from 98.4%to 101.3%(RSD<2.0%,n=6).The RSDs of precision,reproducibility and stability tests(24 h)were lower than 2.0%(n=6).Conclusion:The established method is stable and reliable,which can be used for the content determination of Xinshuning tablets.
作者
印成霞
许凤泉
Yin Chengxia;Xu Fengquan(Dongying Institute for Food and Drug Control,Shandong Dongying 257091,China)
出处
《中国药师》
CAS
2020年第2期373-376,共4页
China Pharmacist
