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目的:建立高效液相色谱-三重四级杆串联质谱(HPLC-QQQ-MS)法同时测定附子理中丸中制附子6种生物碱成分含量的方法。方法:采用Thermo Accucore RP-MS色谱柱(2.1 mm×100 mm,2.6μm),以0.1%甲酸水-0.1%甲酸乙腈为流动相,流速0.3 m L·min-1,柱温30°C。质谱条件:采用电喷雾电离源(ESI),正离子检测模式,扫描方式为多反应离子监测模式(MRM),定量分析离子分别为苯甲酰新乌头碱m/z 105.0,苯甲酰乌头碱m/z 105.0,苯甲酰次乌头碱m/z 542.3,新乌头碱m/z 572.3,乌头碱m/z 586.3,次乌头碱m/z 556.3。结果:苯甲酰新乌头碱、苯甲酰乌头碱、苯甲酰次乌头碱、新乌头碱、乌头碱、次乌头碱线性范围分别在0.184 80~1.848 ng(r=0.999 6),0.035 36~0.353 6 ng(r=0.999 6),0.129 60~1.296 ng(r=0.999 8),0.011 65~0.116 5 ng(r=0.999 8),0.002 95~0.029 5 ng(r=0.999 8),0.036 96~0.369 6 ng(r=0.999 8),6种生物碱的含量在一定范围内线性关系良好(r>0.999 6)。加样回收率在91.93%~106.70%,RSD均<6.00%。结论:该方法简单、准确、灵敏、重复性好,可用于附子理中丸中制附子生物碱成分的含量测定。
OBJECTIVE: To establish a method for the simultaneous determination of six alkaloids in aconite by HPLC-QQQ-MS with high performance liquid chromatography-triple quadrupole mass spectrometry. Methods: The chromatographic column (2.1 mm × 100 mm, 2.6 μm) with 0.1% formic acid and 0.1% formic acid in acetonitrile was used as the mobile phase at a flow rate of 0.3 m L · min-1 and the column temperature was 30 ° C. Mass spectrometry conditions: electrospray ionization source (ESI), positive ion detection mode, scanning mode for multiple reaction ion monitoring mode (MRM), quantitative analysis of ions were benzoyl mesaconitine m / z 105.0, benzoyl Head base m / z 105.0, benzoyl hypaconitine m / z 542.3, mesaconitine m / z 572.3, aconitine m / z 586.3, hypaconitine m / z 556.3. Results: The linear ranges of benzoyl mesaconitine, benzoyl aconitine, benzoyl hypaconitine, mesaconitine, aconitine and hypaconitine were 0.184 80-1.848 ng (r = 0.999 6), 0.035 36 ~ 0.353 6 ng (r = 0.999 6), 0.129 60 ~ 1.296 ng (r = 0.999 8), 0.011 65 ~ 0.116 5 ng = 0.999 8) and 0.036 96 ~ 0.369 6 ng (r = 0.999 8). The contents of six alkaloids were linear within a certain range (r> 0.999 6). The recoveries of samples ranged from 91.93% to 106.70% with RSD <6.00%. Conclusion: The method is simple, accurate, sensitive and reproducible. It can be used for determination of alkaloids in aconite of Fuzi Li Zhong Wan.