固相萃取-高效液相色谱法同时测定水环境中的10种典型PPCPs.docVIP

固相萃取-高效液相色谱法同时测定环境水体中10种典型PPCPs ( （东华大学环境科学与工程学院，上海 201620） 摘要：结合固相萃取与高效液相色谱分析技术，建立了一种可以同时检测环境水体中10种典型PPCPs的分析方法，考察了固相萃取小柱类型、水样pH值、洗脱溶剂种类和洗脱溶剂体积对目标PPCPs萃取回收率的影响，同时对高效液相色谱分离条件进行了优化。结果表明，将水样pH值调节至5，采用Poly-Sery HLB固相萃取小柱对目标PPCPs进行富集，然后使用6 mL的100%甲醇洗脱，经色谱分离测定可知建立的方法曲线在0.5~20 mg·L-1内线性关系良好。对自来水和地表水的加标回收率分别为66.9~108.5%和71.2~108.2%，检测方法的检出限为6.0~54.6 μg·L-1。采用该方法对上海市某城镇污水处理厂的和出水μg·L-1）、四环素（47.1 μg·L-1）和磺胺甲噁唑（119.1 μg·L-1），在处理出水中仅检测出环丙沙星，浓度为4.1 μg·L-1。 关键词：PPCPs; 固相萃取; 高效液相色谱; 环境水体 Simultaneous determination of ten typical pharmaceuticals and personal care products in environmental waters by solid-phase extraction with high-performance liquid chromatography WU Li-le, REN Jin-tao, WANG Kai, XUE Gang, LIU Zhen-hong, GAO Pin* (College of Environmental Science and Engineering, Donghua University, Shanghai 201620) Abstract: A solid-phase extraction (SPE) with high-performance liquid chromatography (HPLC) method has been developed for simultaneous determination of ten typical pharmaceuticals and personal care products (PPCPs) in environmental waters. Effects of SPE cartridge type, sample pH value, eluent type and eluent volume on recovery rate of the target PPCPs were investigated. In addition, the chromatographic separation conditions were optimized as well. The results showed that the linear relationship of the established method within 0.5~20 mg/L was favorable as the optimum conditions for SPE process were as follows: sample pH of 5, SPE cartridge type of the Poly-Sery HLB, eluent with 6 mL of 100% methanol. Moreover, the recoveries of standard addition for portable water and surface water were 66.9~108.5% and 71.2~108.2%, respectively. Limits of detection of the method were in the range of 6.0 to 54.6 μg·L-1. Finally, the method was applied for detection of the target PPCPs in raw influent and final effluent from a sewage treatment plant in Shanghai. The results indicated that ciprofloxacin, tetracycline and sulfamethoxazole were detected in raw influent at 17.9, 47.1 and 119