基于石墨烯固相萃取的液相色谱质谱联用仪对4种四环素类药物检测研究

Drug monitoring study of four tetracyclines by liquid chromatography-mass spectrometry based on graphene solid phase extraction

目的建立基于石墨烯固相萃取前处理的液相色谱质谱联用仪检测四环素的方法。方法样品匀浆后,由石墨烯吸附提取液中的四环素类药物,而后洗脱下来,对提取液pH值、洗脱液的组成进行优化,利用液相色谱质谱联用仪进行检测。结果用pH=4. 5的提取液提取,用纯甲醇作为洗脱液洗脱,可以达到固相萃取最佳的回收率。4种四环素类药物的线性方程R^2均达到0. 995以上,检出限达到2μg/kg以下。结论利用石墨烯进行固相萃取前处理,用液相色谱质谱联用仪进行检测,能够对4种四环素类药物达到满意的检测结果。

Objective To establish a method for the detection of tetracycline by liquid chromatography-mass spectrometry based on the pretreatment of graphene solid phase extraction.Methods After the sample is homogenized,the tetracyclines in the extract are adsorbed by graphene,and then eluted,and the p H of the extract and the composition of the eluate are optimized,and the liquid chromatography-mass spectrometer is used for detection.Results The best recovery rate of solid phase extraction was obtained by extraction with pH 4~5 and eluting with pure methanol.All R^2 of the four tetracycline drugs were above 0.995 and the detection limit was below 2μg/kg.Conclusion Pretreatment with solid phase extraction using graphene and detection by liquid chromatography-mass spectrometry can achieve satisfactory results for four tetracyclines.