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

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 mL甲醇和3 mL水活化,采用5 mL的10%甲醇水溶液作为淋洗液,2 mL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340.4 μg/kg,定量限(LOQ)为1126.8 μg/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)、1532.1 μg/kg。

Quantitative Analysis of Cephalosporin C in Soil by High Performance Liquid Chromatography with Ultrasound-assisted Extraction and Solid-Phase Extraction

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.