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作 者:蔡振世 CAI Zhenshi(Quanzhou Institute For Food And Drug Control,Quanzhou 362000,Fujian,China)
出 处:《市场监管与质量技术研究》2023年第1期13-16,共4页Market Regulation and Quality Technology Research
摘 要:文中建立一种UPLC-MS/MS法同时测定珍菊降压片中可乐定、蒙花苷、绿原酸、氢氯噻嗪、芦丁含量。采用ACQUITY UPLC?BEH柱(C182.1 mm×50 mm1.7μm),以0.1%甲酸水溶液-甲醇为流动相梯度洗脱,流速:0.3 mL·min^(-1),柱温35℃,进样量2μL。质谱采用ESI(电喷雾离子源),以正负离子多反应监测模式定量分析。实验结果显示,可乐定、蒙花苷、绿原酸、氢氯噻嗪、芦丁的线性范围为0.02648~0.8472μg·m L^(-1)、0.1011~3.235μg·m L^(-1)、0.08055~2.578μg·mL^(-1)、0.02600~0.8320μg·mL^(-1)、0.1033~3.306μg·mL^(-1)(r^(2)为0.99167~0.99907),平均加标回收率分别为95.1%、93.2%、91.7%、94.6%、92.8%,RSD为2.81%、2.02%、3.41%、3.15%、1.79%(n=6)。结果表明该方法操作简单、便捷、快速,可一次性实现多个不同成分的检测,结果准确可靠。UPLC-MS/MS method was developed for the simultaneous determination of clonidine, linarin, chlorogenic acid, hydrochlorothiazide and rutin in Zhenjujiangya tablets. Methods of ACQUITY UPLC?BEH column(C18 2.1 mm×50 mm 1.7 μm) will be used with 0.1% formic acid aqueous solution-methanol as mobile phase for gradient elution, in which the flow rate was 0.3 mL·min^(-1), the column temperature was 35 ℃, and the sample volume was 2 μL. ESI(electrospray ionization source) was used in the mass spectrometry to monitor the Quantitative analysis of positive and negative ion multi-reaction mode. The results of the experiment show that the linear ranges of clonidine, linarin,chlorogenic acid, hydrochlorothiazide and rutin were 0.02648 ~ 0.8472 μg·mL^(-1), 0.1011 ~ 3.235 μg·mL^(-1), 0.08055 ~ 2.578 μg·mL^(-1),0.02600 ~ 0.8320 μg·mL^(-1), 0.1033 ~ 3.306 μg·mL^(-1)(r^(2) was 0.99167-0.99907);the average recoveries were 95.1 %, 93.2 %, 91.7 %, 94.6 %,92.8 %;RSD were 2.81 %, 2.02 %, 3.41 %, 3.15 %, 1.79 %(n=6). There comes a conclusion that the method is simple, convenient as well as fast and can detect multiple components at one time. In addition, the results are accurate and reliable.
关 键 词:UPLC-MS/MS 珍菊降压片 蒙花苷 绿原酸 芦丁
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