摘要
建立反相高效液相色谱法快速测定注射用蜂毒中蜂毒肽含量。采用Triart C_(18)色谱柱(150 mm×4.6 mm,3μm)为分离柱,以体积分数为0.1%的三氟乙酸溶液为流动相A、体积分数为0.1%的三氟乙酸乙腈溶液为流动相B进行梯度洗脱,流量为1.0 mL/min,进样体积为10μL,检测波长为220 nm,柱温为30℃。在上述色谱条件下,蜂毒肽主色谱峰与相邻杂质峰能实现有效分离,蜂毒肽的质量浓度在0.063~0.504 mg/mL范围内与色谱峰面积线性关系良好,相关系数为0.999 2,方法检出限为0.2μg/mL,定量限为0.4μg/mL。10次测定结果的相对标准偏为1.9%,样品加标平均回收率为98.3%。该方法可用于注射用蜂毒中蜂毒肽的质量控制。
A method was established for rapid determination of melittin in Toxic Apis for injection by reversed-phase high performance liquid chromatography.Triart C_(18) chromatographic column(150 mm×4.6 mm,3μm)was used as the separation column,with 0.1%trifluoroacetic acid solution as the mobile phase A and 0.1%trifluoroacetic acid acetonitrile solution as the mobile phase B for gradient elution.The flow rate was 1.0 mL/min,the injection volume was 10μL,the detection wavelength was 220 nm,and the column temperature was 30℃.Under the above chromatographic conditions,the main chromatographic peak of melittin ccould be effectively separated from adjacent impurity peaks.The mass concentration of melittin had good linear relationship with the chromatographic peak area in the range of 0.063-0.504 mg/mL,with correlation coefficient of 0.9992.The detection limit of the method was 0.2μg/mL and the quantification limit was 0.4μg/mL.The relative standard deviation of 10 measurement results was 1.9%,and the average recovery of sample spiked was 98.3%.This method can be used for quality control of melittin in Toxic Apis for injection.
作者
苗会娟
徐艳梅
张媛
胡卫国
刘建芬
高燕霞
MIAO Huijuan;XU Yanmei;ZHANG Yuan;HU Weiguo;LIU Jianfen;GAO Yanxia(Hebei Provincial Institute of Drug and Medical Device Inspection,Hebei Province Center for Drug Quality Control and Evaluation Technology Innovation,Shijiazhuang 050020,China;National Institute for Food and Drug Control,Beijing 102629,China;North China Pharmaceutical Huakun Hebei Biotechnology Co.,Ltd.,Shijiazhuang 050000,China)
出处
《化学分析计量》
2026年第1期105-110,共6页
Chemical Analysis And Meterage
基金
2023年度石家庄市“揭榜挂帅”制科技项目(231790153A)。
关键词
蜂毒肽
注射用蜂毒
反相高效液相色谱
melittin
Toxic Apis for injection
reverse phase high performance liquid chromatography
