摘要：目的：不同于传统的高效液相色谱法对药物的分离分析，亚临界水色谱法减少了流动相中有害的有机溶剂，是一种绿色分离技术。所以本论文以酚麻美敏片为实验对象，采用亚临界水色光谱法测定了氢溴酸右美沙芬、对乙酰氨基酚以及马来酸氯苯那敏的含量。方法：样品制备时，取酚麻美敏片1片，研细，加1%乙酸溶液适量后超声20min,然后过滤并定容到50ml。采用石墨碳柱,0.01mol/L硫酸水溶液-乙醇（80:20）为流动相，流速1.0 mL/min,进样体积为5 μL,检测波长为279 nm,柱温为110℃。结果：标样中对乙酰氨基酚线性范围为0.33-20.00 mg/mL（r =0.9944），氢溴酸右美沙芬线性范围为0.033-2.00mg/mL（r =0.9934），马来酸氯苯那敏线性范围为0.0067-0.400mg/mL（r =0.9929），样品中马来酸氯苯那敏、氢溴酸右美沙芬、对乙酰氨基酚的回收率均在均在 97.6% - 101.1%之间。结论：该方法实验操作简单，结果比较准确，适用于该产品的质量控制。

关键字：酚麻美敏片; 对乙酰氨基酚; 马来酸氯苯那敏; 亚临界水色谱法；氢溴酸右美沙芬

Study on pharmaceutical analysis with high performance subcritical liquid chromatography 

Abstract: Purpose: Different from the traditional HPLC method for the separation and analysis of drugs, the sub-critical water chromatography reduces the harmful organic solvents in the mobile phase and becomes a green separation technology. Therefore, the content of dexamethafine hydrobromate, paracetaminophen and chlorpheniramine maleate were determined by subcritical water chromatography using Fen-Ma-Mei-Min tablet as the experimental sample. Method: For the sample preparation, one piece of Fen-Ma-Mei-Min tablet was porphyrized. The sample was extracted with ultrasound 20min in 1% acetic acid solution, then filtrated and fixed volume to 50ml with 1% acetic acid. HPLC analysed using graphite carbon column, 0.01 mol/L sulfuric acid aqueous solution - ethanol (80:20) as mobile phase, flow rate of 1.0 mL/min, sample volume for 5 μL, detection wavelength of 279 nm, column temperature is 110 ℃. Results: The linear relationship was deterrmined for acetaminophen in 0.33-20.00 mg/mL (r = 0.9944), dextromethorphan hydrobromide in 0.033-2.00 mg/mL (r = 0.9934), chlorpheniramine maleate in 0.0067-0.400 mg/mL (r = 0.9929). The recovery rate of all 3 components were between 97.6% and 101.1%. Conclusion: the method is simple, accurate and suitable for the quality control of the product.

KEY WORDS: Phenolamine tablet; Acetaminophen; Chlorphenamine maleate; Subcritical water chromatography；Dextromethorphan hydrobromide

目录

1 前言 1

1.1 选题意义 1

1.2 文献综述 1

1.2.1 亚临界水 1

1.2.2 色谱与亚临界水色谱 1

1.2.3 仪器系统 2

1.2.4 亚临界水色谱应用 2

1.2.5 复方感冒药概述 3

1.2.6 成分及含量分析 4

2 实验内容 6

  2.1 仪器与试剂 6

2.1.1 实验仪器 6

2.1.2 实验试剂 6

2.2 实验方法 6

2.2.1 样品选定 6

2.2.2 样品的制备 7

2.2.3 HPLC检测条件 7

2.3 方法验证