加速溶剂萃取(ASE)-固相萃取(SPE)-高效液相色谱法(HPLC)测定土壤中青霉素钠  

Determination of sodium penicillin in soil through accelerated solvent extraction and solid phase extraction followed by high performance liquid chromatography(ASE-SPE-HPLC)

作　　者：马珊珊[1,2] 刘燕[2] 余冉[1] 张振华[2] 于赐刚[2] 宋海亮[1] 王长永[2] 

机构地区：[1]东南大学能源与环境学院,南京210096 [2]环境保护部南京环境科学研究所,南京210042

出　　处：《环境化学》2014年第11期1978-1985,共8页Environmental Chemistry

基　　金：环境保护部环保公益性行业科研专项(201209024);江苏省青年自然科学基金(BK21030102)资助

摘　　要：建立了一种加速溶剂萃取(ASE)-固相萃取(SPE)-高效液相色谱(HPLC)测定土壤中青霉素钠的简单、快速的方法.样品以超纯水为提取溶剂,50℃提取温度为ASE提取条件参数;HLB型固相萃取柱富集净化:6.0mL 5%甲醇淋洗、4.0mL乙腈-甲醇(1∶1)洗脱;高效液相色谱-紫外检测器(HPLC-PDA)测定,检测波长λ=191.1nm,柱温30℃,流动相为乙腈-0.1%甲酸/水(1∶1),采用等梯度洗脱程序,取得较好的检测分离效果.对0.5、2.0、8.0mg·kg-1等3个不同添加浓度水平的青霉素钠平均加标回收率范围为73.1%—89.7%,回收率相对标准偏差RSD范围为1.1%—2.9%(n=5),检出限可达235.0μg·L-1.结果表明,该方法操作简单,快速,准确度和精密度均符合质量控制要求,能够满足环境土壤样本中痕量青霉素钠检测分析的要求.A rapid and simple method based on accelerated solvent extraction,solid-phase extraction followed by high performance liquid chromatography（ ASE-SPE-HPLC） was proposed for the determination of sodium penicillin in soil. The optimum pre-treatment parameters for the soil samples contaminated with sodium penicillin are as follow： ultra-pure water as extraction solvent for penicillin,50 ℃ extraction temperature,HLB as solid phase extraction cartridges,6. 0 m L 5%methanol as rinse solvent,4. 0 m L acetonitrile and methanol（ 1 ∶ 1） as eluent followed by detection with HPLC-PDA. The results also showed that when acetonitrile and 0. 10% formic acid（ 1 ∶ 1）,30 ℃ column temperature,191. 1 nm detection wavelength were applied during gradient mobile process,HPLC assay offered a good potential for the sensitive and selective determination of sodium penicillin. The average recovery rate for three different treatments was 73. 1% —89. 7% under the optimized pre-treatment and detection parameters,and the precision was 1. 1% —2. 9%（ n = 5）.Furthermore,the detection sensitivity for sodium pencillin in soil reached 235. 0 μg·L- 1. In conclusion,ASE-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 sodium penicillin in various soilsamples.

关 键 词：青霉素钠 加速溶剂萃取 固相萃取 高效液相色谱 

分 类 号：X833[环境科学与工程—环境工程] O657.72[理学—分析化学]