【摘要】目的:采用HPLC法測定己酮可可堿葡萄糖注射液中5-羥甲基糠醛限量。方法:ODSC18柱(250×4.6 mm,5 μm),以甲醇:水:三乙胺(50:50:0.1)為流動相,檢測波長為284 nm。結(jié)果:回歸方程A=4100.91+53467.52C (r=0.999,n=5),在濃度1 μg/ml~20 μg/ml的范圍內(nèi)線性良好,加樣回收率為99.89 %,RSD=0.19 %。結(jié)論:本方法準確而靈敏,能有效地控制5-羥甲基糠醛的限量。
【關(guān)鍵詞】 己酮可可堿葡萄糖注射液 5-羥甲基糠醛 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
己酮可可堿為一種甲基黃嘌呤類血管擴張劑,臨床用于缺血性腦血管疾病、血管性頭痛和血栓閉塞性脈管炎的治療。己酮可可堿葡萄糖注射液為含己酮可可堿和5%葡萄糖的滅菌水溶液。其中葡萄糖降解產(chǎn)物5-羥甲基糠醛(5-HMF)的控制是重要的質(zhì)量指標,限度應(yīng)不低于中國藥典中葡萄糖注射液的限度要求。但按照文獻[1]方法采用分光光度法于284 nm處直接測定5-HMF時,由于己酮可可堿在此波長有最大吸收,對測定產(chǎn)生干擾。故本研究采用高效液相色譜法測定己酮可可堿葡萄糖注射液中5-HMF的限量,以提高檢測的準確度及靈敏度醫(yī)學全.在.線m.52667788.cn。
1 儀器與試藥
高效液相色譜儀:SSITP420 檢測器型號: SSI500DETECTOR Variable UV/VIS 己酮可可堿 :上海申興藥廠提供(批號:20000105) 5-HMF對照品:美國Sigma公司提供(批號:H9877) 己酮可可堿葡萄糖注射液 :南京小營制藥廠提供(批號:00052001、00052002、00052003) 甲醇(色譜純) 三乙胺(分析純)
2 結(jié)果
2.1 色譜條件
色譜柱:十八烷基硅烷鍵合硅膠250 mm×4.6 mm 流動相為甲醇:水:三乙胺(50:50:0.1) 流速:1.0 ml/min 檢測波長:284 nm。