【摘要】目的:采用HPLC法测定己酮可可碱葡萄糖注射液中5-羟甲基糠醛限量。方法:ODSC18柱(250×4.6 mm,5 μm),以甲醇:水:三乙胺(50:50:0.1)为流动相,检测波长为284 nm。结果:回归方程A=4100.91+53467.52C (r=0.999,n=5),在浓度1 μg/ml~20 μg/ml的范围内线性良好,加样回收率为99.89 %,RSD=0.19 %。结论:本方法准确而灵敏,能有效地控制5-羟甲基糠醛的限量。
【关键词】 己酮可可碱葡萄糖注射液 5-羟甲基糠醛 HPLC Determination of 5-hidroxymethylfurfural in pentoxifylline and glucose injection by HPLC WANG Ji-rong (The Nanjing Childrens Hospital Affiliated to Nanjing Medical University, Jiangsu Nanjing 210008,China) Abstract: Objective To determine 5-HMF in pentoxifylline and glucose injection. Methods C18 (250 mm×4.6 mm) column with methanol:water:triethylamine (50:50:0.1) as mobile phase was used. The detection wave-length was 284nm. Results The caliPation curves of 5-hydroxymethylfurfural was linear in range of 1 μg/mL~20 μg/mL. The average recovery was 99.89 %,(RSD=0.19 %).Conclusion The method is specific and reliable for the determination of 5-HMF in pentoxifylline and glucose injection. Key words: Pentoxifylline and glucose injection;5-HMF;HPLC
己酮可可碱为一种甲基黄嘌呤类血管扩张剂,临床用于缺血性脑血管疾病、血管性头痛和血栓闭塞性脉管炎的治疗。己酮可可碱葡萄糖注射液为含己酮可可碱和5%葡萄糖的灭菌水溶液。其中葡萄糖降解产物5-羟甲基糠醛(5-HMF)的控制是重要的质量指标,限度应不低于中国药典中葡萄糖注射液的限度要求。但按照文献[1]方法采用分光光度法于284 nm处直接测定5-HMF时,由于己酮可可碱在此波长有最大吸收,对测定产生干扰。故本研究采用高效液相色谱法测定己酮可可碱葡萄糖注射液中5-HMF的限量,以提高检测的准确度及灵敏度医学全.在.线www.lindalemus.com。
1 仪器与试药
高效液相色谱仪:SSITP420 检测器型号: SSI500DETECTOR Variable UV/VIS 己酮可可碱 :上海申兴药厂提供(批号:20000105) 5-HMF对照品:美国Sigma公司提供(批号:H9877) 己酮可可碱葡萄糖注射液 :南京小营制药厂提供(批号:00052001、00052002、00052003) 甲醇(色谱纯) 三乙胺(分析纯)
2 结果
2.1 色谱条件
色谱柱:十八烷基硅烷键合硅胶250 mm×4.6 mm 流动相为甲醇:水:三乙胺(50:50:0.1) 流速:1.0 ml/min 检测波长:284 nm。