色谱

色谱 ›› 2013, Vol. 31 ›› Issue (2): 133-138.DOI: 10.3724/SP.J.1123.2012.09023

• 研究论文 • 上一篇    下一篇

pH/溶剂双梯度反相高效液相色谱法同时测定氨酚曲麻片中的5种有效成分

禤学怡, 黄丽娜, 潘晓玲, 李宁*   

  1. 广东药学院, 广东 广州 510006
  • 收稿日期:2012-09-17 修回日期:2012-11-15 出版日期:2013-02-28 发布日期:2013-02-05
  • 通讯作者: 李宁
  • 基金资助:

    国家自然科学基金项目(81173525).

Simultaneous determination of five cold medicine ingredients in paracetamol triprolidine hydrochloride and pseudoephedrine hydrochloride tablets by pH/organic solvent double-gradient high performance liquid chromatography

XUAN Xueyi, HUANG Lina, PAN Xiaoling, LI Ning*   

  1. Guangdong College of Pharmacy, Guangzhou 510006, China
  • Received:2012-09-17 Revised:2012-11-15 Online:2013-02-28 Published:2013-02-05

PDF

332

被引次数

12

摘要： 建立了一种pH/溶剂双梯度反相高效液相色谱(HPLC)同时测定氨酚曲麻片中对乙酰氨基酚、咖啡因、水杨酰胺、盐酸伪麻黄碱、盐酸曲普利啶5种有效成分的方法。通过对溶剂梯度和pH/溶剂双梯度体系的优化,得到分离5种成分的最佳色谱体系。采用Diamonsiol C18色谱柱(250 mm×4.6 mm, 5 μm),以甲醇、0.05 mol/L醋酸铵水溶液和0.08 mol/L醋酸水溶液组成三元流动相体系,pH/溶剂双梯度洗脱,流速为1.0 mL/min;柱温为30 ℃。采用分段变波长检测: 0～6 min, 280 nm; 6～7 min, 257 nm; 7～14 min, 280 nm; 14 min, 233 nm。片剂中的5种成分在25.5 min内能达到基线分离,对乙酰氨基酚、盐酸伪麻黄碱、咖啡因、水杨酰胺、盐酸曲普利啶5种成分的线性范围分别为0.055～0.998 g/L、0.053～0.946 g/L、0.007～0.129 g/L、0.035～0.622 g/L和0.002～0.039 g/L,相关系数r均大于0.9990;检出限(以信噪比为3(S/N=3)计)分别为0.09、6、0.02、0.128和0.02 mg/L,回收率为97.9%～102.8%。该方法能在短时间内同时分离酸性、中性和碱性化合物,能提高被测物的柱效,减少半峰宽和拖尾,可应用于氨酚曲麻片中5种成分的含量分析。

关键词: pH/溶剂双梯度, 氨酚曲麻片, 对乙酰氨基酚, 高效液相色谱法, 咖啡因, 水杨酰胺, 盐酸曲普利啶, 盐酸伪麻黄碱

Abstract: A pH/organic solvent double-gradient mode in reversed-phase high performance liquid chromatography (HPLC) has been established as a new approach to the simultaneous determination of acetaminophen, caffeine, salicylamide, pseudoephedrine hydrochloride and triprolidine hydrochloride in paracetamol triprolidine hydrochloride and pseudoephedrine hydrochloride tablets. Through the optimization of the organic solvent gradient mode and pH/organic solvent double-gradient mode, the optimum double-gradient HPLC system of the five cold medicine ingredients has been built. The determination was carried out on a Diamonsiol C18 column (250 mm×4.6 mm, 5 μm). The mobile phase consisted of methanol, 0.05 mol/L ammonium acetate solution and 0.08 mol/L acetic acid solution. The column temperature was set at 30 ℃. The flow rate was 1.0 mL/min. The sample was measured at multiple wavelengths: 0-6 min, 280 nm; 6-7 min, 257 nm; 7-14 min, 280 nm; 14 min, 233 nm. The separation of the five cold medicine ingredients in the tablets was achieved in 25.5 min. The linear ranges of acetaminophen, pseudoephedrine hydrochloride, caffeine, salicylamide and triprolidine hydrochloride were 0.055-0.998 g/L, 0.053-0.946 g/L, 0.007-0.129 g/L, 0.035-0.622 g/L and 0.002-0.039 g/L, respectively, with their correlation coefficients greater than 0.9990. The detection limits (S/N=3) were 0.09, 6, 0.02, 0.128 and 0.02 mg/L, respectively. Their mean recoveries were 97.9%-102.8%. The advantage of the method is the simultaneous determination of acidic, neutral and basic compounds. It also can improve the column efficiency of the analyte, compress the half-peak width and reduce the trailing. The optimized and validated method can be used for the simultaneous determination of the five cold medicine ingredients in the tablets.

Key words: acetaminophen, caffeine, high performance liquid chromatography (HPLC), paracetamol triprolidine hydrochloride and pseudoephedrine hydrochloride tablets, pseudoephedrine hydrochloride, salicylamide, triprolidine hydrochloride, pH/organic solvent double-gradient