[关键词]
[摘要]
目的 建立同时测定乙肝宁颗粒中10种指标成分的UPLC方法,为乙肝宁颗粒的质量控制提供科学依据。方法 采用UPLC-DAD法,色谱柱为Acquity UPLC BEH C18(100 mm×2.1 mm,1.7 μm);流动相为乙腈-甲醇-0.15%磷酸水溶液,梯度洗脱,体积流量0.3 mL/min,柱温45℃,进样量2 μL。结果 同时测定了乙肝宁颗粒中绿原酸、白术内酯I、芍药苷、毛蕊异黄酮苷、二苯乙烯苷、咖啡酸、川楝素、山柰素、丹皮酚、丹参酮ⅡA 10种有效成分,各成分在考察的质量浓度范围内线性关系良好(r≥0.999 0),检测限与定量限分别为0.006~0.017 μg/mL和0.017~0.510 μg/mL,平均加样回收率为98.8%~102.5%,RSD为1.13%~5.37%。通过对16个批次样品的测定,上述10种成分的平均质量浓度依次为(5.724±0.017)、(0.273±0.003)、(0.854±0.005)、(1.228±0.004)、(0.496±0.003)、(1.287±0.004)、(0.137±0.004)、(3.624±0.014)、(7.366±0.032)、(1.754±0.005)mg/g。结论 所建立的UPLC方法简单、专属、灵敏,可用于乙肝宁颗粒质量控制和评价。
[Key word]
[Abstract]
Objective To establish a UPLC method to simultaneously determine 10 active ingredients in Yiganning Granules (YG) and provide scientific basis for the quality control, evaluation and standard revision of YG preparations. Methods A UPLC method was used with an Acquity UPLC BEH C18 column (100 mm×2.1 mm, 1.7 μm). The mobile phase was acetonitrile-mehanol-0.15% phosphoric acid solution with gradient elution. The flow rate was 0.3 mL/min. The column temperature was 45 ℃. The injection volume was 2 μL. Results Ten active ingredients (chlorogenic acid, atractylenolide I, paeoniflorin, calycosin 7-O-β-D- glucopyranoside, stilbene glycoside, caffeic acid, toosendanin, kaempferol, paeonol and tanshinone ⅡA) in YG were simultaneously determined. The linearity was good (r ≥ 0.999 0), the limit of detection and quantification were 0.006—0.017 μg/mL and 0.017—0.510 μg/mL. The average recoveries were 98.8%—102.5% with RSDs of 1.13%—5.37%. Through the determination of 16 batches of samples, the average content of the above 10 ingredients was in turn (5.724±0.017), (0.273±0.003), (0.854±0.005), (1.228±0.004), (0.496±0.003), (1.287±0.004), (0.137±0.004), (3.624±0.014), (7.366±0.032) and (1.754±0.005) mg/g, respectively. Conclusion The established UPLC method is simple, specific, sensitive, stable, precise, accurate, and reproducible, which can be used for quality control and evaluation of YG.
[中图分类号]
R286.02
[基金项目]
天津市科技计划项目(No.18YFZCSY00015)