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目的建立了梯度洗脱高效液相色谱(RP-HPLC)法测定长春西汀葡萄糖注射液中5-羟甲基糠醛含量的分析方法。方法以Agilent C18(250 mm×4.6 mm,5μm)为色谱柱,考察了不同流动相的等度和梯度洗脱法,优化后的方法以0.2 mol/L醋酸铵为水相,乙腈为有机相进行梯度洗脱,检测波长为284 nm,流速为1.0 ml/min。结果该法5-羟甲基糠醛(5-HMF)在0.0021μg/ml~21.37μg/ml范围内浓度与峰面积的线性关系良好,检测限为0.64 ng/ml,平均回收率为98.5%。该法分别测定了6家企业的样品以及室温放置(60 d)、强光照射(10 d)、高温60℃(10 d)、115℃(20 min)灭菌、121℃(20 min)灭菌等条件下降解的5-羟甲基糠醛的含量。结论该法专属性强,准确度高,在检测长春西汀葡萄糖注射液中降解产物5-HMF的同时,也避免了大浓度的长春西汀长时间地吸附在色谱柱上。
Objective To establish a method for the determination of 5-hydroxymethylfurfural in Vinpocetine Injection by gradient elution high performance liquid chromatography (RP-HPLC). Methods The isocratic and gradient elution methods of different mobile phases were investigated on an Agilent C18 (250 mm × 4.6 mm, 5 μm) column. The optimized method consisted of 0.2 mol / L ammonium acetate as the aqueous phase and acetonitrile as the organic phase Gradient elution was performed with a detection wavelength of 284 nm and a flow rate of 1.0 ml / min. Results The linear range of 5-HMF was 0.0021μg / ml ~ 21.37μg / ml. The detection limit was 0.64 ng / ml and the average recovery was 98.5%. The method was used to determine the samples of six enterprises, which were sterilized at 115 ℃ (20 min) and 121 ℃ (20 min) after being exposed to light (10 d), 60 ℃ (10 d) Degradation of 5-hydroxymethyl furfural content of bacteria and other conditions. Conclusion The method is highly specific and accurate. It can avoid the adsorption of large concentrations of vinpocetine on the column for a long time while detecting the degradation product 5-HMF in vinpocetine glucose injection.