UPLC-MS/MS法同时测定沙参麦冬汤中9种成分的含量
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篇名: UPLC-MS/MS法同时测定沙参麦冬汤中9种成分的含量
TITLE:
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5 μl。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4.14×105 Pa,加热气压力为4.48×105 Pa,帘气压力为1.72×105 Pa,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。
ABSTRACT: 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 4.14×105 Pa, heater pressure was 4.48×105 Pa, curtain air was 1.72×105 Pa, 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.
期刊: 2016年第27卷第9期
作者: 吴茵,王蕊,任炳楠,孙源,刘勇,张黎媛
AUTHORS: WU Yin,WANG Rui,REN Bingnan,SUN Yuan,LIU Yong,ZHANG Liyuan
关键字: 超高效液相色谱-串联质谱法;沙参麦冬汤;定量;多反应监测模式
KEYWORDS: UPLC-MS/MS; Shasheng maidong decoction; Quantification; Multiple reaction monitoring model
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