建立了以硝酸钾作为背景电解质测定阿霉素脂质体药物中微量硫酸根离子的毛细管电泳分析法。考察了分离电压、背景电解质、电渗流改性剂浓度、pH值对分离测定的影响。结果表明,当毛细管长度为60cm(有效长度51.5cm)、分离电压为-15kV、缓冲溶液采用20mm o l/L硝酸钾(pH7.0)、电渗流改性剂采用0.4mm o l/L十六烷基三甲基氯化铵(CTAC)、检测波长为202nm时,阿霉素脂质体破乳液中硫酸根离子和氯离子在3m in内得到了基线分离,硫酸根离子迁移时间和峰面积的相对标准偏差分别小于0.01%和1.0%,检出限为5μg/L。用该方法对阿霉素脂质体样品中的微量硫酸根离子进行了分析测定,结果令人满意。
A capillary electrophoretic method for the determination of the trace sulfate ion in liposome doxorubicin has been developed with potassium nitrate as the background electrolyte.The components and pH of the buffer solution,the concentration of electroosmotic flow modifier and the separation voltage on the separation were studied in detail.The optimized electrophoretic conditions were as follows: capillary column diameter 50 μm,total length 60 cm and effective length 51.5 cm,20 mmol/L potassium nitrate buffer solution(pH 7.0) containing 0.4 mmol/L cetyltrimethylammonium chloride(CTAC) as the electroosmotic flow modifier,an applied voltage of-15 kV(reversed polarity) and a detection wavelength of 202 nm.Under the optimized capillary electrophoresis separation conditions,sulfate ion and chloride ion in the liposome doxorubicin breaking emulsion were separated successfully within 3 min,and the relative standard deviations of migration time and peak area of sulfate ion were less than0.01% and 1.0% respectively.The detection limit was 5 μg/L.This method has been proved to be simple,sensitive and accurate,and also has been applied to determine sulfate ion in liposome doxorubicin sample with satisfactory results.