引用本文
  •    [点击复制]
  •    [点击复制]
【打印本页】 【下载PDF全文】 查看/发表评论下载PDF阅读器关闭

←前一篇|后一篇→

过刊浏览    高级检索

本文已被:浏览 1964次   下载 1936 本文二维码信息
码上扫一扫!
超高效液相色谱结合亲水相互作用色谱法测定普鲁卡因青霉素注射液中普鲁卡因和青霉素的含量
吴剑平,姜芹,王博,严凤,张文刚,黄士新
0
(上海市兽药饲料检测所)
摘要:
建立了超高效液相色谱结合亲水相互作用色谱法测定普鲁卡因青霉素注射液中的主成分含量的方法。精密量取1.00 mL样品悬浊液置分液漏斗中,加入石油醚和甲醇震摇提取。静置分层后将下层提取液取出置容量瓶中以甲醇定容至刻度。提取液经稀释至适当浓度后过0.22 μm滤膜,上机测定。目标物使用超高效液相色谱等度洗脱分离。以亲水相互作用色谱柱为固定相, 以0.05 mol/L甲酸铵溶液( pH=4.00):乙腈=10: 90为流动相。紫外二级管阵列检测器检测235 nm波长处吸收进行定量分析。实验结果表明,该方法在青霉素含量40 mg/mL~800 mg/mL,普鲁卡因含量50 mg/mL~1000 mg/mL内线性关系良好(r >0.999),其添加回收率在92 %~105 %,RSD<3 %,表明该方法具有较好的准确度与精密度。通过与《中国兽药典2015版一部》注射用普鲁卡因青霉素含量测定项下方法所测得结果的比较,两者RSD<3 %,表明结果一致。
关键词:  普鲁卡因  青霉素  超高效液相色谱  亲水相互作用色谱
DOI:
投稿时间:2019-12-19修订日期:2020-03-27
基金项目:
Determination of Procaine Benzylpenicillin for Injection by Ultra Performance Liquid Chromatogram with Hydrophilic Interaction Chromatography Method
(Shanghai Municipal Supervisory Institute Veterinary Drugs and Feedstaff)
Abstract:
To determine procaine benzylpenicillin for injection, an UPLC method combined with HILIC was established. 1.00 mL sample was accurately measured to a separating funnel, petroleum ether and methanol was added to extract the sample. After standing and demixed, the lower layer was transferred to a volumetric flask and filled with methanol to scale. The extract was diluted to a proper concentration and filtered by 0.22 μm film, then injected. The targets were separated by isocratic elution with UPLC. The stationary phase was HILIC column, and the mobile phase was 0.05 mol/L ammonium formate solution ( pH=4.00): acetonitrile= 90: 10. The UV diode array was set to 235 nm to achieve the quantitation. The results showed that the method was with good linearity(r >0.999) in the range of 40 mg/mL~800 mg/mL with benzylpenicillin and 50 mg/mL~1000 mg/mL with procaine. The recovery were between 92% ~ 105% and the RSD were lower than 3%, which showed the good accuracy and precision of the method. The results were compared to those measured by the determination of procaine benzylpenicillin for injection from china veterinary pharmacopoeia. The results were in agreement with the RSD were lower than 3%.
Key words:  Procaine  benzylpenicillin  UPLC  HILIC

用微信扫一扫

用微信扫一扫