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.
关键词
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/MSShasheng maidong decoctionQuantificationMultiple reaction monitoring model