高效液相色谱法同时测定甲磺酸双氢麦角碱注射液中3种单碱和总碱的含量

Determination of content of the three alkaloids and the total alkaloid in dihydroergotoxine methanesulfonate injection by HPLC

目的:建立用高效液相色谱法(HPLC)同时测定甲磺酸双氢麦角碱注射液中3种单碱和总碱的含量方法。方法:采用HPLC法,C18色谱柱(150mm×4.6mm,5μm);流动相:乙腈-水-三乙胺(30∶70∶2.0);检测波长:280nm。结果:单碱Ⅰ在0.406～4.06μg之间线性关系良好,r=0.9998,平均回收率为98.49%,RSD为1.23%;单碱Ⅱ在0.406～4.06μg之间线性关系良好,r=0.9998,平均回收率为100.55%,RSD为3.29%;单碱Ⅲ在0.406～4.06μg之间线性关系良好,r=0.9998,平均回收率为98.73%,RSD为5.21%;总碱在1.22～12.18μg·mL-1之间线性关系良好,r=0.9998,平均回收率为98.08%,RSD为1.26%。结论:HPLC法同时测定甲磺酸双氢麦角碱注射液中3种单碱和总碱的含量专属性强,灵敏度高,准确性好,可用于甲磺酸双氢麦角碱注射液含量测定。

OBJECTIVE To determine the three kinds of alkaloid and the total alkaloid in dihydroergotoxine methanesulfonate injection by HPLC. METHODS HPLC was used. C18 column （250 mm × 4. 6mm, 5 μm） was selected, the mobile phase was acetonitrile-H2O- triethylamine（30：70：2. 0）. Detection was performed by UV with wavelength of 280 nm. RESULTS A linearity of alkaloid Ⅰ was obtained from 0. 406 to 4. 06μg with good correlation（r = 0. 999 8）. The average recovery of alkaloid Ⅰ was 98. 49%, and RSD was 1.23%. A linearity of alkaloid Ⅱ was obtained from 0. 406 to 4. 06 μg with good correlation（r= 0. 999 8）. The average recovery of alkaloid Ⅱ was 100. 55%, and RSD was 3. 29%. A linearity of alkaloid Ⅲ was obtained from 0. 406 to 4. 06μg with good correlation（r= 0. 999 8）. The average recovery of alkaloid Ⅲ was 98. 73%, and RSD was 5.21%. A linearity of the total alkaloid was obtained from 1.22 to 12. 18 μg with good correlation（r= 0. 999 8）. The average recovery of the total alkaloid was 98. 08%, and RSD was 1.26%. CONCLUSION The HPLC is sensitive and accurate in determining the three kinds of alkaloid and the total alkaloid in dihydroergotoxine methanesulfonate injection. It can be applied efficiently.