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作 者:宋更申[1,2] 周丽[3] 徐艳梅 张西如 张兰桐[1]
机构地区:[1]河北医科大学,河北石家庄050017 [2]河北省药品检验研究院,河北石家庄050011 [3]石药集团中奇制药技术(石家庄)有限公司,河北石家庄050041
出 处:《药学学报》2016年第5期792-796,共5页Acta Pharmaceutica Sinica
基 金:河北省自然科学基金资助项目(H2012206079)
摘 要:建立UPLC-ESI-MS/MS法测定八子补肾胶囊中14种成分的含量。Waters ACQUITY BEH C18柱(50mm×2.1 mm,1.7μm),柱温为40℃;流动相为A(乙腈)-B(0.1%乙酸),梯度洗脱;电喷雾离子源(ESI源),源温度为150℃,毛细管电压为2.0 k V,离子源补偿电压为50 V,脱溶剂气温度为500℃,脱溶剂气流量为800 L·h^(-1),锥孔气流量为150 L·h^(-1),雾化气压力为7.0 Bar(1 Bar=100 k Pa),接口处加热,采用多反应监测模式。在本方法条件下,14种成分的线性关系良好(r^2≥0.999 1),定量限为0.11~4.52 ng·m L^(-1)。精密度为0.8~2.1%。平均回收率范围为97.89%~101.9%。该方法操作简便、快速、准确度高、重现性好,可用于八子补肾胶囊的质量控制。The study developed a method for the determination of 14 components in Bazibushen capsule by UPLC-ESI-MS/MS.Waters ACQUITY BEH C18 column(50 mm × 2.1 mm,1.7 μm) was used and the column temperature was 40 ℃.A linear gradient elution of eluents A(acetonitrile) and B(0.1% acetic acid) was used for the separation.The source temperature was set at 150 ℃.The capillary voltage was set at 2.0 k V.The source offset voltage was kept at 50 V.The desolvation temperature was set at 500 ℃.The desolvation flow was 800 L·h^-1.The cone flow was 150 L·h^-1.The nebuliser pressure was 7.0 Bar.Multiple reaction monitoring mode(MRM) is adopted.All of the 14 components showed good linearity(r^2 〉0.999 1) in the test ranges.The LOQs for the compounds ranged from 0.11-4.52 ng·mL^-1,respectively.The RSDs were 0.8%-2.1%.The overall recoveries were between 97.89% and 101.9% for all compounds.The method is simple,rapid,accurate and highly reproducible,and may be used in the determination of 14 components in Bazibushen capsule.
关 键 词:八子补肾胶囊 含量测定 UPLC-ESI-MS/MS
分 类 号:R917[医药卫生—药物分析学]
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