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作 者:邹准[1] 闵建国[1] 吴敏菊[1] 钟小清[1] 周艳林[1] 邹节明[1] ZOU Zhun;MIN Jian-guo;WU Min-ju;ZHONG Xiao-qing;ZHOU Yan-lin;ZOU Jie-ming(Guilin Sanjin Pharmaceutical Co.,Ltd.,Guilin 541004,China)
机构地区:[1]桂林三金药业股份有限公司,广西桂林541004
出 处:《中草药》2021年第14期4217-4220,共4页Chinese Traditional and Herbal Drugs
基 金:广西创新驱动发展科技重大专项(桂科AA17202045)。
摘 要:目的建立一种高效液相色谱-电喷雾检测器(HPLC-CAD)法分离测定三金片中积雪草苷B和羟基积雪草苷2个同分异构体含量的方法。方法采用Thermo Acclaim^(TM) C_(30)色谱柱,甲醇-乙腈-水(35∶8∶57)为流动相,柱温35℃,CAD气化温度为50℃,采集频率为10 Hz,分离测定积雪草苷B和羟基积雪草苷的含量。结果积雪草苷B和羟基积雪草苷线性关系良好,r分别为0.999 8、0.998 4,线性范围分别为0.240 7~2.406 9、0.573 1~5.730 8μg,平均加样回收率分别为100.26%、98.32%,RSD分别为0.69%、1.78%;11批样品中积雪草苷B为1.65~3.18 mg/g,羟基积雪草苷为3.49~7.90mg/g。结论该方法简便、灵敏、准确度高,能有效分离测定积雪草苷B和羟基积雪草苷2个同分异构体,可用于三金片现行药典标准的提高完善。Objective To establish a HPLC-CAD method for the determination of asiaticoside B and madecassoside in Sanjin Tablets(三金片). Methods The separation was performed on Thermo Acclaim^(TM) C_(30) column(250 mm × 4.6 mm, 5μm) with the mobile phase of methanol-acetonitrile-water(35∶8∶57). The flow rate was 1.0 mL/min and the column temperature was 35 ℃. CAD detection condition included that the nebulization temperature was 50 ℃ and data acquisition frequency was 10 Hz. The content of asiaticoside B and madecassoside was determinated. Results The linear ranges of asiaticoside B and madecassoside were 0.240 7—2.406 9 μg(r = 0.999 8) and 0.573 1—5.730 8 μg(r = 0.998 4), respectively. The average recoveries of asiaticoside B and madecassoside were 100.26%(RSD 0.69%) and 98.32%(RSD 1.78%), respectively. The contents of asiaticoside B and madecassoside in 11 batches of samples were 1.65—3.18 mg/g and 3.49—7.90 mg/g. Conclusion The method is accurate, convenient and sensitive for the quality control of two isomers(asiaticoside B and madecassoside) in Sanjin Tablets.
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