摘要
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 A gradient elution - HPLC method was developed for 5 - HMF content analysis in vinpocetine and glu- cose injection. Methods Agilent C18 （250 mm × 4.6 mm, 5 μm） was used as the chromatographic column, the acetonitrile - 0.2 mol/L ammonium acetate solution was used as mobile phase for gradient elution at a flow rate of 1.0 ml/min, and the de- tection wavelength was 284nm. Results The method showed good linearity between concentration and peak area in the range of 0. 0021 μg/ml ~21.37 μg/ml for 5 - HMF. The detection limit was 0.64 ng/ml. The average recovery （ n = 9） of 5 - HMF was 98.5%. The contents of 5 - HMF were determined in samples from six companies and degraded samples at room tempera- ture for60 d, with highlight for 10 d, with high temperature at60 ℃for 10 d, at 115 ℃ for20 min, at 121 ℃ for20 min re- spectively. Conclusion The method had strong specificity and high accuracy, and it can avoid the long - time adsorption of the large - concentration vinpocetine on chromatographic column in determination of 5 - HMF in vinpocetine and glucose injection.
出处
《中国卫生检验杂志》
北大核心
2014年第6期824-825,828,共3页
Chinese Journal of Health Laboratory Technology
