【摘要】 建立了一种采用超声辅助提取(UAE)、强阴离子交换固相萃取(SAX-SPE)净化、高效液相色谱(HPLC)测定土壤中残留头孢菌素C(CPC)简单、快速方法。样品以超纯水为提取剂,超声辅助提取,SPE柱子以3 m L甲醇和3 m L水活化,采用5 m L的10%甲醇水溶液作为淋洗液,2 m L的5%甲酸水溶液/甲醇溶液(体积比50∶50)进行洗脱,高效液相色谱紫外检测器(HPLC-PDA)测定,检测波长λ=254 nm,柱温30℃,流动相为0.1%甲酸水溶液/甲醇溶液(体积比95∶5)对土壤中不同加标浓度的CPC进行检测,方法的回收率在77.9%~98.9%,标准偏差范围为5.0%~6.3%(n=5),方法检出限(LOD)为340.4μg/kg,定量限(LOQ)为1126.8μg/kg。同时采用此方法检测分析新疆某药厂附近阳性土壤样品,不同批次土壤样品结果分别为:检出(低于定量限)、1532.1μg/kg。更多还原

【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 m L 10% methanol as rinse solvent,2. 0 m L 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,and254 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.更多还原