离子对反相高效液相色谱梯度洗脱法分析测定硫酸博莱霉素  

Analysis and Determination for Components of Bleomycin Sulfate by Ion - Pair RP - HPLC Gradient Elution Method

作　　者：周明昊[1] 

机构地区：[1]浙江省药品检验所,杭州310004

出　　处：《药物分析杂志》2002年第2期114-117,共4页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:研究应用反相离子对色谱梯度洗脱法以较快速度分离硫酸博莱霉素组分,并尝试梯度洗脱条件下测定其有效成分A_2、B_2的含量。方法:色谱柱为八烷基硅烷键合硅胶柱(4.6mm×150 mm,填料:Eclipse XDB,粒度:5μm),检测波长为254nm,采用甲醇-庚烷磺酸钠溶液为流动相进行梯度洗脱(甲醇起始比例为30％,35 min内上升至40％),流速为1.2mL·min^(-1),柱温为30℃,进样量为10μL。结果:博莱霉素A_2、B_2、A_5、B_4、去甲基A_2等组分在此条件下基本实现基线分离,A_2、B_2在0.1～2.0 mg·mL^(-1)范围内,浓度与峰面积均呈良好线性关系(r均为0.999 9)。结论:本法可在较短时间内使博莱霉素组分得到良好分离。Objective: To develop a HPLC linear gradient elution method for rapid separation of the components of bleomycin, and for determination of bleomycin A2 and bleomycin B2. Method; Eclipse XDB - C8 column (4. 6 mm ×150 mm, 5 uuuum) with temperature at 30℃was used with a mobile phase of methanol and sodium heptane-sulfonate solution, use a linear gradient of 30% to 40% methanolic solution of sodium heptanesulfonate in 35 minutes, allow chromatography to proceed with the final gradient mixture for a further 5 minutes. The elution was performed at the flow rate of 1. 2 mL· min-1. UV detection wavelength is 254 nm. Result: Components of bleomycin , especially bleomycin A2 , bleomycin B2 , bleomycin A5 , bleomycin B4 , demethyl bleomycin A2 were separated successfully . The calibration curves for bleomycin A2 and bleomycin B2 were linear in the range of 0. 1 -2.0 mg·mL-1 respectively . Conclusion: This method is rapid, accurate and reproducible.

关 键 词：离子对-反相高效液相色谱 博莱霉素 梯度洗脱 硫酸博莱霉素 测定 抗肿瘤抗生素 

分 类 号：R979.14[医药卫生—药品]