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一种改进的SPE-HPLC法用于水中多环芳烃的测定
Determination of PAHs in Water by Improved SPE-HPLC Method
【摘要】 采用流动相乙腈-水梯度洗脱的高效液相色谱方法,使得标准溶液16种多环芳烃(PAHs)得到了完全分离,线性相关系数均达到0.999以上,相对标准偏差均在3%以内,检出限均在0.02~8 ng/L范围内。通过设计实验确定了固相萃取空白干扰的存在,萘和菲干扰明显,玻璃器皿、橡胶管和室内环境均可能带来干扰。研究了有机改进剂甲醇含量和加标方式对空白加标回收率的影响,结果显示10%甲醇含量和标准溶液先加入甲醇再加入水中超声的加标方式,多环芳烃具有较高的回收率80.6%~121.3%。比较了氮吹和水浴旋蒸的不同浓缩方式对溶剂加标回收率的影响,发现水浴旋蒸较氮吹不会带来干扰外,还具有较高的回收率。应用上述确定的条件测定实际样品地表水和地下水,发现均有0~12.1 ng/L不同程度的检出。
【Abstract】 A method of HPLC with gradient elution of mobile phase acetonitrile-water was developed,by which 16 PAHs standard solution was completely separated,the linear correlation coefficients being above 0.999,the relative standard deviations less than 3%,and the limits of detection within the range of 0.02 to 8 ng/L. The blank interferences during solid phase extraction were found through the experiment,i.e. naphthalene and phenanthrene interference significantly,glassware,rubber tubing and indoor environment were likely to bring about interference. Furthermore,the influences of content of organic modifier methanol and spike mode on spike-recovery were investigated,and the results showed that when 10%methanol solution that was added into the standard solution then added to the water with ultrasound treatment,polycyclic aromatic hydrocarbons would have high recovery rates(80.6% ~121.3%). In addition,the effect of different concentrated manners on spike-recovery was studied by nitrogen blowing and rotary evaporation,it was found that rotary evaporation would not cause interference,on the contrary,had a high recovery. In conclusion,with the above identified testing condition PAHs detected in the real samples of both surface water and groundwater were with the range of 0~12.1 ng/L.
【Key words】 polycyclic aromatic hydrocarbons(PAHs); high performance liquid chromatography(HPLC); solid phase extraction; organic modifier; spike recovery;
- 【文献出处】 环境科学与技术 ,Environmental Science & Technology , 编辑部邮箱 ,2016年09期
- 【分类号】X832
- 【被引频次】2
- 【下载频次】220