全自动固相膜萃取-高效液相色谱法测定水源水中的16种多环芳烃  

Determination of polycyclic aromatic hydrocarbons in source water by automatic solid phase membrane extraction and high-performance liquid chromatography

作　　者：冯晓青[1] 邢亚东[1] 汪怡 王芹[1] 王露[1] 宋鑫[1] 徐瑞[1] 杭学宇[1] 

机构地区：[1]淮安市疾病预防控制中心,江苏淮安223001

出　　处：《现代预防医学》2018年第3期501-505,共5页Modern Preventive Medicine

基　　金：淮安市科技支撑计划(社会发展)项目(HAS2015030);江苏省卫生计生委预防医学科研项目(Y2015033)

摘　　要：目的建立全自动固相膜萃取结合高效液相色谱法测定水源水中的16种多环芳烃。方法水样加入10%甲醇后上样,上样流速为100 ml/min,待测物经固相膜萃取后,采用二氯甲烷进行洗脱,浓缩后上机,梯度洗脱,C_(18)色谱柱分离,DAD检测器检测,根据保留时间和峰面积进行定性定量分析。从色谱条件、溶剂置换条件和萃取液浓缩方式等对水中16种PAHs的全自动固相膜萃取-液相色谱方法进行了优化研究。结果在0.05μg/ml^5.0μg/L范围内,相关系数r>0.999;16种多环芳烃的仪器检出限为0.28 ng/L^1.04 ng/L;对水源水样品进行3个浓度水平0.05μg/L、0.5μg/L和5.0μg/L,平均回收率在29.4%~100.3%之间;相对标准偏差(RSD)为2.3%~9.2%。结论本法自动化程度高,快速、灵敏、简单,适用于快速分析环境水样中的痕量多环芳烃。Objective To establish a method of automatic solid - phase membrane extraction and high - performance liquid chromatography determination of sixteen polycyclic aromatic hydrocarbons in source water. Methods After adding 10% methanol, the sample solution was extracted with the solid - phase membrane, eluted and concentrated with methylene chloride, and the enriched samples were determined. The separation of samples was performed on a C18 column by gradient elution using acetonitrile and water as mobile phase. The samples were separated and detected with photodiode array detector （ DAD ）. The qualification analysis was performed by retention time and UV spectrum, and the quantification analysis was based on the peak area. Results Calibration curves were obtained at a concentration range of 0.05 - 5.0μg/ml with correlation coefficient r 〉 0. 999. The method quantification limits ranged from 0.28 ng/L - 1.04 ng/L. The average recoveries at 3 spiked levels of 0.05, 0.5 and 5.0 μg/L were ranged from 29.4 % to 100.3 %, and the relative standard deviations （RSD） were in the range of 2.3 % - 9.2%. Conclusion This method is automated, simple, rapid, sensitive, repeatable, reliable and suitable for determination of polycyclic aromatic hydrocarbons in water.

关 键 词：固相膜萃取 高效液相色谱法 多环芳烃 水源水 

分 类 号：R115[医药卫生—公共卫生与预防医学]