摘要
目的：建立同时测定沙参麦冬汤中芦丁、甘草苷、补骨脂素、花椒毒素、佛手苷内酯、甘草酸铵、麦冬皂苷D、甲基麦冬二氢高异黄酮A、甲基麦冬二氢高异黄酮B含量的方法。方法：采用超高效液相色谱-串联质谱法。色谱柱为Phenomenex Kinetex C18,流动相为乙腈-0.1%甲酸（梯度洗脱）,流速为0.3 ml/min,柱温为25℃,进样器温度为10℃,平衡时间为2 min,进样量为5μl。离子化模式为电喷雾电离,源喷射电压分别为5 500 V、-4 500 V,雾化气压力为4.14×10-5Pa,加热气压力为4.48×10^-5Pa,帘气压力为1.72×10^-5Pa,离子源温度为650℃,工作模式为多反应监测模式。结果：芦丁、甘草苷、补骨脂素、花椒毒素、佛手苷内酯、甘草酸铵、麦冬皂苷D、甲基麦冬二氢高异黄酮A和甲基麦冬二氢高异黄酮B的检测质量浓度线性范围分别为1.75-700、5.00-1 997、0.95-380、1.75-700、2.00-800、7.00-2 799、2.38-950、0.38-151、0.43-171 ng/ml（r为0.999 2、0.999 7、0.999 0、0.999 1、0.999 8、0.999 3、0.999 5、0.999 7、0.999 0）;精密度、稳定性、重复性试验的RSD≤3.0%;加样回收率分别为98.76%-107.60%、92.57%-105.80%、92.30%-103.10%、93.20%-108.10%、94.62%-99.20%、95.08%-104.80%、95.71%-104.80%、94.54%-105.50%、94.50%-103.00%,RSD分别为1.7%、2.9%、2.1%、3.0%、1.2%、2.6%、1.9%、2.3%、1.6%（n=6）。结论：该方法快速、简便、准确可靠,适用于同时测定沙参麦冬汤中9种成分的含量。
OBJECTIVE：To establish a method for the contents determination of rutin,liquiritin,psoralen,xanthotoxin,bergapten,ammonium glycyrrhetate,ophiopogonin D,methylophiopogonanone A and methylophiopogonanone B in Shasheng maidong decoction. METHODS：UPLC-MS/MS was conducted. The column of UPLC was Phenomenex Kenetix C18 with mobile phase of acetonitrile solution-0.1% formic acid（gradient elution）at a flow rate of 0.3 ml/min,the column temperature was 25 ℃,injector temperature was 10 ℃,equilibrium time was 2 min and the injection volume was 5 μl. Ionization mode was electrospray ionization with spray voltage of 5 500 V and-4 500 V,atomizing air pressure was 4.14×10-5Pa,heater pressure was 4.48×10^-5Pa,curtain air was 1.72×10^-5Pa,and the ion source temperature was 650 ℃,the work mode was multiple reaction monitoring mode. RESULTS：The linear range was 1.75-700 ng/ml（r=0.999 2）for rutin,5.00-1 997 ng/ml（r=0.999 7）for liquiritin,0.95-380 ng/ml（r=0.999 0）forpsoralen,1.75-700 ng/ml（r=0.999 1）for xanthotoxin,2.00-800 ng/ml（r=0.999 8）for bergapten,7.00-2 799 ng/ml（r=0.999 3）for ammonium glycyrrhetate,2.38-950 ng/ml（r=0.999 5）for ophiopogonin D,0.38-151 ng/ml（r=0.999 7）for methylophiopogonanone A,and 0.43-171 ng/ml（r=0.999 0）for methylophiopogonanone B;RSDs of precision,stability and reproducibility tests were no more than 3.0%;recoveries were 98.76%-107.60%（RSD=1.7%）,92.57%-105.80%（RSD=2.9%）,92.30%-103.10%（RSD=2.1%）,93.20%-108.10%（RSD=3.0%）,94.62%-99.20%（RSD=1.2%）,95.08%-104.80%（RSD=2.6%）,95.71%-104.80%（RSD=1.9%）,94.54%-105.50%（RSD=2.3%）and 94.50%-103.00%（RSD=1.6%）,respectively（n=6）. CONCLUSIONS：The method is rapid,simple,accurate and reliable,and suitable for 9 ingredients in Shasheng maidong decoction.
出处
《中国药房》
CAS
北大核心
2016年第9期1240-1244,共5页
China Pharmacy
基金
河北省医学科学研究重点课题计划(No.ZL20140340)
河北省中医药类科研计划课题(No.2014152)
