应用化学2018，Vol.35Issue(6)：722-728,7.DOI:10.11944/j.issn.1000-0518.2018.06.170245
超声辅助提取-固相萃取土壤中头孢菌素C的高效液相色谱法定量检测
Quantitative Analysis of Cephalosporin C in Soil by High Performance Liquid Chromatography with Ultrasound-assisted Extraction and Solid-Phase Extraction
摘要
Abstract
A rapid and simple method based on ultrasound-assisted extraction, solid-phase extraction followed by high performance liquid chromatography ( UAE-SPE-HPLC ) was proposed for the determination of cephalosporin C( CPC) in soil.The optimum pre-treatment parameters for the soil samples contaminated with CPC are as follow: ultra-pure water as extraction solvent for CPC, SPE as solid phase extraction cartridge, 5.0 mL 10%methanol as rinse solvent, 2.0 mL 5%formic acid/methanol solution( volume ratio 50:50) as eluent.The results show that when 0.1%formic acid and methanol(95:5) , 30 ℃column temperature, and 254 nm detection wavelength were applied during the isocratic elution process, HPLC assay offeres a good potential for the sensitive and selective determination of CPC.The recovery rates for seven different treatments are 77.9%~98.8%, and the precision is 5.0%~6.3%( n=5) .The limit of determination( LOD) and the limit of quantification( LOQ) in soil are 340.4 μg/kg and 1126.8 μg/kg, respectively.At the same time, this method was used to detect the positive soil near the pharmaceutical factory in Xinjiang.The experimental results of different batches show detected ( below LOQ ) , 1532.1 μg/kg and detected ( below LOQ ) , respectively.In conclusion, UAE-SPE-HPLC is simple and rapid.Its accuracy and precision are in line with the quality control requirements.It is suitable for the detection of trace CPC in soil.关键词
头孢菌素C/土壤/超声辅助提取/固相萃取/高效液相色谱Key words
cephalosporin C/soil/ultrasound-assisted extraction/solid-phase extraction/high performance liquid chromatography分类
化学化工引用本文复制引用
王悦,蔡辰,刘惠玲,孙丽,李彦超,孟昭虹..超声辅助提取-固相萃取土壤中头孢菌素C的高效液相色谱法定量检测[J].应用化学,2018,35(6):722-728,7.基金项目
国家自然科学基金(41401589)、黑龙江省自然科学基金、黑龙江省高校大学专项科研资金项目(HDRCCX-2016Z10)资助 Supported by the National Natural Science Foundation of China(No.41401589), the Natural Science Foundation of Heilongjiang Province, Special Research Funds for the Universities of Heilongjiang Province(No.HDRCCX-2016Z10) （41401589）
