脉络宁注射液中5-羟甲基糠醛、绿原酸和咖啡酸的含量测定及安全性分析

Determination and Safety Analysis of 5-Hydroxymethyl Furfural,Chlorogenic Acid and Caffeic Acid in Mailuoning Injection

目的测定79批脉络宁注射液中5-羟甲基糠醛、绿原酸和咖啡酸的含量,并对这3种既有效又可能导致不良反应成分的安全性作出分析。方法色谱柱为Agilent Zorbax SB-C18（4.6 mm×150 mm,5μm）;流动相为甲醇-0.1%甲酸,梯度洗脱;DAD检测,定量波长5-羟甲基糠醛为283 nm,绿原酸和咖啡酸为325 nm;柱温为20℃。结果 5-羟甲基糠醛、绿原酸和咖啡酸的含量分别为0.15%~0.41%（RSD=19.34%）、0.03%~0.07%（RSD=15.83%）和0.02%~0.05%（RSD=18.88%）,平均含量分别为0.28%、0.05%和0.03%。结论从79批测定数据来看,本制剂中5-羟甲基糠醛、绿原酸及咖啡酸的含量均波动较大,其中5-羟甲基糠醛平均含量达到0.28%,参照葡萄糖类注射液有关标准,此含量偏高,可能存在一定的安全风险。

OBJECTIVE To assay three components,which are effective but potentially cause ADRs,in 79 batches of Mailuoning Injections in order to conduct a safety analysis on the injection.METHODS The HPLC method was used for the analysis,the experiment was carried out on an Agilent Zorbax SB-C18 column（4.6 mm×250 mm,5 μm） in a gradient elution with the mobile phase of MeOH-0.1% formic acid solution.DAD was used for detection,and the quantitative wavelength was set at 283 nm for 5-hydroxymethyl furfural and 325 nm for chorogenic acid and caffeic acid respectively.The column temperature was 20 ℃.RESULTS In 79 batches of samples,5-hydroxymethyl furfural,chorogenic acid and caffeic acid were in the range of 0.15%-0.41%（RSD=19.34%）,0.03%-0.07%（RSD=15.83%） and 0.02%-0.05%（RSD=18.88%）,with average value of 0.28%,0.05% and 0.03%,respectively.CONCLUSION The results showed that the variability of three components contained in 79 batches of samples were fluctuated to some extent.The mean of 5-hydroxymethyl furfural reached 0.28% that could have potential riskness in use,based on the limitation of 0.02% required in the standard of glucose injection.