摘要
目的:建立同时测定桑菊感冒丸中芦丁、连翘苷和桔梗皂苷D含量的方法。方法:采用高效液相色谱-串联质谱法。色谱柱为Waters Atlantis C_(18),流动相为乙腈-0.1%甲酸溶液(梯度洗脱),流速为0.2 mL/min,柱温为35℃,进样量为10μL。离子源为电喷雾离子源,采用多反应监测扫描模式和正离子检测模式,干燥气和雾化气均为高纯氮气,干燥气温度为270℃,干燥气流量为25 L/min,鞘气流量为10 L/min,毛细管电压为4 500 V,喷嘴电压为2 000 V,扫描时间为0.1 s。结果:芦丁、连翘苷和桔梗皂苷D检测质量浓度线性范围分别为0.010 82~2.164μg/mL(r=0.999 7)、0.010 18~2.036μg/mL(r=0.999 4)、0.010 27~2.054μg/mL(r=0.999 7);定量限分别为1.250、0.260、2.720 ng/mL,检测限分别为0.380、0.078、0.820 ng/mL;精密度、稳定性、重复性试验的RSD<3.0%;加样回收率分别为97.88%~99.88%(RSD=0.72%,n=6)、98.48%~103.13%(RSD=1.91%,n=6)、98.79%~101.41%(RSD=1.05%,n=6)。结论:该方法操作简便,精密度、稳定性、重复性好,可用于桑菊感冒丸中芦丁、连翘苷和桔梗皂苷D含量的同时测定。
OBJECTIVE： To establish the method for simultaneous determinations of rutin, forsythin and platycodin D in Sangju ganmao pills. METHODS： HPLC-MS method was adopted. The determination was performed on Waters Atlantis C18 column with mobile phase consisted of acetonitrile-0.1% formic acid （gradient elution） at the flow rate of 0.2 mL/min. The column temperature was set 35 ℃, and sample size was 10 μL. The ionization mode was electrospray ion, and the reaction mode was multi-reaction monitoring. By positive ion detection mode, the drying gas and nebuliser gas were all high purity nitrogen. The drying gas temperature was 270 ℃.The drying gas flow rate was 25 L/min. The sheath gas flow rate was 10 L/min. The capillary voltage was 4 500 V. The nozzle voltage was 2 000 V and the scanning time was 0.1 s. RESULTS： The linear range of rutin, forsythin and platycodin D were 0.010 82-2.164 μg/mL （r=0.999 7）, 0.010 18-2.036 μg/mL （r=0.999 4）,0.010 27-2.054 μg/mL （r=0.999 7）, respectively. The limits of quantification were 1.250,0.260,2.720 ng/mL, and the limits of detection were 0.380,0.078, 0.820 ng/mL. RSDs of precision, stability and reproducibility tests were all no more than 3.0%. The recoveries were 97.88%-99.88% （RSD=0.72%,n=6）,98.48%-103.13%（RSD=1.91%,n=6）, 98.79%-101.41%（RSD=1.05%,n=6）. CONCLUSIONS： This method is simple, precise, stable and reproducible, and can be used for simultaneous determination of rutin, forsythin and platycodin D in Sangju ganmao pills.
出处
《中国药房》
CAS
北大核心
2017年第36期5163-5166,共4页
China Pharmacy
