Objective : To establish a HPLC-MS method for determining of three kind of diester diterpenoid alkaloids in the guifudihuang pills. Method : HPLC-MS was used. The separation was performed on Polaris C18 -A (50 mm ×2.0 mm, 5 μm) column with the mobile phase of CH3OH - H2O(90 : 10) , The flow rate is 0. 2 ( mL· min -1) . The detection was done by positive-ion electrospray ionization mass spectrometry. Results : The linear ranges are 46. 4 - 278. 4 ( ng · mL -1) ( r = 0.9995) for mesacontine, 6. 8-108. 8 ( ng· mL-1) ( r =0. 9998) for aconitine and 48.2 - 771. 2 ( ng · mL-1) ( r = 0. 9997) for hypaconitine respectively. The average recoveries ( n = 6) were 97. 9％ ( RSD = 3.0％) for mesacontine, 98.2％ ( RSD = 3. 2 ％ ) for aconitine and 97. 6％ ( RSD = 3.0％) for hypaconitine respectively.Conclusion: A rapid, sensitive and accurate method for the determination of mesacontine,aconitine and hypaconitine in the guifudihuang pills was founded. The study may provide a scientific basis for the quality control of guifudihuang pills.%目的:建立测定桂附地黄丸中新乌头碱、乌头碱和次乌头碱的高效液相色谱-质谱分析方法(HPLC-MS).方法:采用HPLC-MS,色谱柱为Polaris C18-A(50 mm ×2.0 mm,5 μm),流动相为甲醇-水(90:10),流速为0.2(mL·min-1),质谱检测采用电喷雾电离源正离子检测.结果:新乌头碱、乌头碱和次乌头碱浓度分别在46.4～278.4(ng·mL-1)(r=0.999 5)、6.8～108.8(ng·mL-1)(r=0.999 8)和48.2～771.2(ng·mL-1)(r=0.999 7)范围内线性关系良好,平均回收率(n=6)分别为97.9%(RSD=3.0%)、98.2%(RSD=3.2%)和97.6%(RSD=3.0%).结论:该法是一种快速、灵敏、准确的分析方法,可为桂附地黄丸的质量控制提供科学依据.
展开▼
