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机构地区:[1]天津医院,天津300180 [2]天津医科大学药学院,天津300070 [3]天津中新药业集团股份有限公司第六中药厂,天津300401 [4]南开大学药学院,天津300071
出 处:《中国药学杂志》2013年第3期216-219,共4页Chinese Pharmaceutical Journal
摘 要:目的建立同时测定舒脑欣滴丸中尿苷、鸟苷、阿魏酸、藁本内酯、洋川芎内酯I和H含量的液相色谱-质谱联用方法(UPLC-Q-TOF)。方法采用Waters Acquity BEH C18色谱柱(2.1 mm×100 mm,1.7μm),流动相为乙腈-甲酸-水体系梯度洗脱,流速为0.4 mL.min-1,PDA检测190~400 nm扫描;进样量:2.0μL。结果尿苷、鸟苷、阿魏酸、藁本内酯、洋川芎内酯I和H分别在10.31~206.24,3.28~65.52,6.36~127.24,8.24~164.88,10.18~200.52,3.14~62.72μg.mL-1内与峰面积呈良好线性关系;精密度、重复性和稳定性良好;加样回收率在99%~101%之间。结论所建立的UPLC-Q-TOF方法简便、准确、快速、重复性好,可用于舒脑欣滴丸中尿苷、鸟苷、阿魏酸、藁本内酯、洋川芎内酯I和H的含量测定,为该药的质量控制提供依据。ABSTRACT : OBJECTIVE To establish an LC-MS method for simultaneous determination of six compounds ( uridine, guanosine, ferulic acid, ligustilide, senkyunolide I and H in Shunaoxin dropping pills. METHODS The analysis was performed on a Waters Aequity BEH Cls column (2. 1 mm × 100 mm, 1.7 μm)with the mixture of acetonitrile-water-formic acid as the mobile phase, and the flow rate was 0. 4 mL · min^-l ; the PDA detection wavelength was 190 -400 nm; the column temperature was room temperature (30 ℃ ). RESULTS The linear ranges for uridine, guanosine, ferulic acid, ligustilide, senkyunolide I and H were 10. 31 -206. 24, 3.28 - 65.52,6. 36 - 127.24,8.24 - 164. 88,10. 18 - 200. 52, and 3.14 - 62. 72μg · mL^-1, respectively. The average recoveries were between 99%-101% (n=6). CONCLUSION This method is simple, accurate and reliable to determine the contents of the six compounds in Shunaoxin dropping pills for the quality control. KEY WORDS : Shunaoxin dropping pill ; LC-MS ; UPLC ; Q-TOF-MS ; ligustilide ; senkyunolide I
关 键 词:舒脑欣滴丸 液相色谱-质谱联用 超高压液相色谱 串联四级杆飞行时间质谱 藁本内酯 洋川芎内酯I
分 类 号:R917[医药卫生—药物分析学]
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