摘要
目的:建立GC-MS法同时测定麝香保心丸中龙脑、异龙脑、肉桂醛、肉桂酸、麝香酮、苯甲酸苄酯6种活性成分的含量。方法:采用气相色谱-质谱联用(GC-MS)法,色谱柱为DB-5(30 m×0.25 mm,0.1μm)毛细管柱;程序升温:70℃恒温2 min,以5℃·min^(-1)的速率升温至150℃,维持4 min,以20℃·min^(-1)的速率升温至260℃,维持3 min;检测质荷比范围:10~425。结果:龙脑、异龙脑、麝香酮、苯甲酸苄酯、肉桂醛、肉桂酸分别在0.022~22.000μg·ml^(-1)(r=0.999 6),0.024~24.000μg·ml^(-1)(r=0.999 6),0.028~28.000μg·ml^(-1)(r=0.999 8),0.034~34.000μg·ml^(-1)(r=0.999 6),0.040~40.000μg·ml^(-1)(r=0.999 7),0.050~50.000μg·ml^(-1)(r=0.999 9)范围内与峰面积呈良好的线性关系。龙脑、异龙脑、肉桂醛、肉桂酸、麝香酮、苯甲酸苄酯的平均加样回收率分别为97.20%,97.40%,97.53%,99.60%,98.78%和98.27%,RSD分别为0.89%,1.18%,1.52%,1.49%,0.79%和1.74%(n=6)。结论:该方法准确、有效、重复性好,可用于麝香保心丸多成分的质量控制研究。
Objective： To develop a GC-MS method for the simultaneous determination of six active constituents（ borneol,isoborneol,cinnamaldehyde,cinnamic acid,muscone and benzyl benzoate） in Shexiang Baoxin pills. Methods： A gas chromatography-mass spectrography（ GC-MS） method was adopted using a DB-5 capillary column（ 30 m×0.25 mm,0.1 μm）. The column temperature was raised as the following program： the initial temperature was 70℃,maintained for 2 min,raised the temperature（ 5℃ ·min^（-1）） to 150℃,maintained for 4 min and then raised the temperature（ 20℃ ·min^（-1）） to 260℃,and maintained for 3 min. The range of mass-to-electric charge ratio was 10 to 425. Results： The calibration curves of borneol,isoborneol,cinnamaldehyde,cinnamic acid,muscone and benzyl benzoate were linear within the range of 0.022-22.000 μg·ml^（-1）（ r= 0.999 6）,0.024-24.000 μg·ml^（-1）（ r =0.999 6）,0.028-28.000 μg·ml^（-1）（ r = 0.999 8）,0.034-34.000 μg·ml^（-1）（ r = 0.999 6）,0.040-40.000 μg·ml^（-1）（ r = 0.999 7） and0.050-50.000 μg·ml^（-1）（ r = 0.999 9）,respectively. The average recovery was 97.20%,97.40%,97.53%,99.60%,98.78% and98.27% and RSD was 0.89%,1.18%,1.52%,1.49%,0.79% and 1.74%（ n = 6）,respectively. Conclusion： The method is accurate,suitable,convenient and reproducible,which can be used for the quality control of multi components in Shexiang Baoxin pills.
出处
《中国药师》
CAS
2016年第4期678-680,共3页
China Pharmacist
