论文部分内容阅读
目的:建立HPLC-ELSD法测定薄芝糖肽注射液中间体中葡萄糖、蔗糖、半乳糖和甘露糖的含量。方法:采用高效液相色谱法测定。色谱条件:色谱柱为Agilent NH_2(150 mm×4.6 mm,5μm),流动相为乙腈-水(84∶16),流速为1.0 m L·min~(-1),柱温为20℃,使用蒸发光散射检测器检测,漂移管的温度为105℃,载气流速为2.0 m L·min~(-1),进样量为10μL。结果:甘露糖、葡萄糖、半乳糖、蔗糖进样量分别在10.088~126.100μg(r=0.990 6),2.118~26.475μg(r=0.999 3),9.302~116.275μg(r=0.995 8),1.874~23.425μg(r=0.999 8)范围内,质量对数与峰面积呈良好的线性关系;平均加样回收率分别为100.43%,100.63%,102.13%,103.82%;RSD分别为2.28%,2.57%,3.16%,1.87%。结论:所建立的方法简便、准确、重现性好,可用于薄芝糖肽注射液中间体中4种游离糖成分的含量测定。
OBJECTIVE: To establish a HPLC-ELSD method for the determination of glucose, sucrose, galactose and mannose in the injection of Boshi glycopeptide. Methods: The determination by high performance liquid chromatography. The chromatographic conditions were as follows: Agilent NH_2 (150 mm × 4.6 mm, 5 μm), mobile phase of acetonitrile-water (84:16), flow rate of 1.0 mL · min -1 and column temperature of 20 ℃ Evaporative light scattering detector detection, the drift tube temperature was 105 ℃, the carrier gas flow rate of 2.0 m L · min -1, the injection volume of 10μL. Results: The injection volumes of mannose, glucose, galactose and sucrose were 10.088-126.100μg (r = 0.9906), 2.118-26.475μg (r = 0.999 3), 9.302-116.275μg (r = 0.995 8), 1.874 ~ 23.425μg (r = 0.999 8), the logarithm of mass showed a good linear relationship with the peak area. The average recoveries were 100.43%, 100.63%, 102.13% and 103.82%, respectively. The RSDs were 2.28% and 2.57 %, 3.16%, 1.87%. Conclusion: The established method is simple, accurate and reproducible. It can be used to determine the contents of four free sugars in the injection of.