石墨烯纳米磁颗粒固相萃取液相色谱质谱联用仪联用法对四环素类药物检测研究

Study on the determination of tetracycline drugs by solid phase extraction(spe) with liquid chromatography and mass spectrometry(lc/ms) of graphene nanoparticles

目的建立石墨烯纳米磁颗粒固相萃取-液相色谱质谱联用对四环素类药物的检测方法。方法取石墨烯、无水硫酸亚铁等试剂,在一定条件下合成石墨烯纳米磁颗粒,对畜禽产品的提取液中四环素类药物进行富集、除杂质、洗脱,进入液相色谱质谱仪进行测定。结果将待测物匀浆于p H=4.5的提取液中,石墨烯纳米磁颗粒吸附3 min,磁铁吸附,弃去提取液,用5%甲醇水溶液除杂质,用纯甲醇洗脱,上机测定,回收率达到90%以上,检出限达到0.2 mg/kg以下,与HLB固相萃取小柱前处理方法比较,检测结果接近。结论石墨烯纳米磁颗粒固相萃取-液相色谱质谱法测定畜禽产品中的4种四环素类药物,与传统HLB小柱方法相比,无需离心机、无需过柱装置、操作简便、成本更低,具有广阔的应用前景。

Objective To establish a method for the determination of tetracycline drugs by solid phase extraction(spe)with liquid chromatography and mass spectrometry(lc/ms)of graphene nanoparticles.Methods Graphene,anhydrous ferrous sulfate and other reagents were used to synthesize graphene nano-magnetic particles under certain conditions.Tetracycline drugs were enriched in the extracts of livestock and poultry products with the nano-magnetic particles.Results The analyte was homogenized in the extract with p H=4.5,the graphene nano-magnetic particles were adsorbed for 3 min,the magnet was adsorbed,the extract was discarded,the impurities were removed with 5%methanol aqueous solution,and eluted with pure methanol.The recovery rate is above 90%,and the detection limit is below 0.2 mg/kg.Compared with the HLB solid phase extraction cartridge pretreatment method,the detection results are close.Conclusion Compared with the traditional HLB small-column method,the method of solid phase extraction with graphene nanoparticles and liquid chromatography-mass spectrometry for the determination of four tetracycline drugs in livestock and poultry products has the advantages of simple operation,low cost and wide application prospect without centrifuge and column crossing device.