解析电喷雾质谱法对感冒药中对乙酰氨基酚的快速检测

Rapid Detection of Paracetamol in Cold Tablets by Desorption Electrospray Ionization Mass Spectrometry

基于常压质谱的直接、快速、无需样品预处理检测的优势,该文拓展了其在药物质检领域的应用。采用自行搭建的解析电喷雾(DESI)装置,对常用感冒药对乙酰氨基酚片进行快速质谱检测,无需样品预处理,直接获得药片中有效成分的分子结构信息。为克服基质差异对定量分析的影响,以淀粉为基质构建对乙酰氨基酚模拟药片,在优化的基础上进行定量实验。针对实际药片中高浓度对乙酰氨基酚检测的需要,研究了其在较高浓度范围的定量关系,结果显示,方法对0.35~4.52 mg/mm^2范围内的对乙酰氨基酚具有较好的线性关系(r^2=0.9982),定量下限为1.903 ng/mm^2,检出限为0.237 ng/mm^2,加标回收率为102%~114%。对3种市售的对乙酰氨基酚片进行直接检测,与厂家提供的标准数据相比,相对标准偏差(RSD)为7.2%~12%,表明方法具有较好准确度。该工作很好地证明了DESI-MS在药品快检中的优势,从而为药品质检提供了潜在的高效、可靠的检测手段。

Based on the advantages of ambient mass spectrometry in the fast and direct detection on samples without any pre-treatment,an ambient mass spectrometric method was developed for the rapid and direct detection of drug tablets.In the experiment,a home-made desorption electrospray ionization(DESI)device was fabricated for the fast mass spectrometry(MS)detection of commercial paracetamol tablets for the cold,achieving the molecule structural information of tablets without any pre-treatment.In the quantitative analysis of tablets by DESI-MS,the tablets of standard paracetamol were made starch used as the main matrix to avoid the effect of matrix on ionizations.Under the optimized conditions,this method was applied in the quantitative detection of paracetamol in real tablets.Results showed that there was a good linear relationship for paracetamol in the range of 0.35-4.52 mg/mm^2 with a correlation coefficient(r^2)of 0.9982.The limit of quantitation and limit of detection were 1.903 ng/mm^2 and 0.237 ng/mm^2,respectively.The spiked recoveries for paracetamol were in the range of 102%-114%.The method was used for the direct detection of paracetamol in three commercial paracetamol tablets.Compared with the data provided by the pharmaceutical manufacturers,the relative standard deviations(RSD)of 7.2%-12%were obtained.The present work confirmed that,with the advantages of drugs rapid detection,DESI-MS provided an efficient and effective tool for quality control of drugs.