高效液相色谱法测定硫酸长春新碱的有关物质

目的 对硫酸长春新碱的有关物质检测方法进行方法学考察.方法 色谱柱为Shiseido C8柱(250 mm×4.6 mm,5μm);取二乙胺15mL加水985 mL,用磷酸调pH至7.5,作为流动相A,甲醇为流动相B,梯度洗脱;流速1.5 mL/min;检测波长297 nm;柱温30℃.结果 6份样品主峰和杂质峰峰面积的RSD分别为0.14%和0.24%;已知杂质硫酸长春碱质量浓度在0.510～51.04μg/mL范国内(相当于杂质水平0.05%~5.O%)与峰面积呈良好的线性关系(r=0.9999);平均加样回收率为100.10%.RSD为0.92%(n=6);有关物质(以硫酸长春碱计)检测限为0.05%.结论 该法专属性、重复性良好,方法准确,检测灵敏度高,耐用性好.可用于原料变更后的产品质量控制.

Determination of Related Compounds of Vincristine Sulfate by HPLC

Objective To study on the method of the related compounds of vincristine sulfate by HPLC. Methods The analytical column was Shiseido C8（250 mm ×4. 6 mm,5 μm）,with column temperature of 30℃. The mobile phase was composed of diethylamine of 15 mL with 985 mL water,adjusted pH to 7.5 by phosphate as A,methanol as B. Detected by gradient elution. Detection wavelength was 297 nm and flow rate of 1.5 mL/min. Results The Intra-day precision RSD was low at 0. 14% ,0. 24%. The linear range of impurities was 0. 510 -51.04 μg/mL（equal to 0. 05% -5.0% of impuritites, r =0. 999 9）. The average recovery was 100. 10% , RSD = 0.92% （n =6）. The lowest detected limits of impurities （detected by vinblastin sulfate） was 0.05%. Conclusions The method is specific, sensitive, accurate, reproducible, stabilitily and suitable for quality control of vineristine sulfate.