饮用水中16种多环芳烃的高效液相色谱-荧光-二极管阵列同时测定法  

Simultaneous determination of 16 polycyclic aromatic hydrocarbons in drinking water with high performance liquid chromatography combine fluorescence detector and diode array detector

作　　者：余辉菊[1] 周琛[2] 

机构地区：[1]成都市疾病预防控制中心理化中心实验室,四川成都610041 [2]四川大学华两公共卫生学院

出　　处：《环境与健康杂志》2016年第2期149-152,共4页Journal of Environment and Health

基　　金：四川省科技支撑计划项目子课题(2012SZ0198)

摘　　要：目的建立饮用水中16种多环芳烃（PAHs）的高效液相色谱-荧光-二极管阵列（HPLC-FLD-DAD）同时测定法。方法将1 L水样经Bond Elut Plexa固相萃取柱吸附,二氯甲烷和乙酸乙酯洗脱,洗脱液经氮吹后用乙腈定容至0.5 ml,经0.45μm滤膜过滤,用Pursuit PAHs色谱柱分离,柱温30℃;用乙腈-水作流动相梯度洗脱,流速为1.8 ml/min;FLD采用波长切换方式测定萘、苊、菲、芴、蒽、荧蒽、芘、苯并[a]蒽、苯并[b]荧蒽、苯并[k]荧蒽、苯并[a]芘、二苯并[a,h]蒽、苯并[g,h,i]苝、茚并[1,2,3-cd]芘15种PAHs,DAD采用254 nm波长检测苊烯;进样体积为5.0μl。结果在0.000 5-100 mg/L的线性范围内,16种PAHs的回归方程均呈较好的线性关系（r〉0.998）。本方法的检出限为0.04-0.50 ng/L,定量下限为0.13-1.67 ng/L;日内和日间RSD分别为1.0%-3.1%和1.5%-3.8%;加标回收率为77.7%-96.9%,加标RSD为1.1%-4.2%。结论该方法快速、准确、灵敏,适用于饮用水中16种PAHs的测定。Objective To develop a method of high performance liquid chromatography（HPLC） combining fluorescence detector（FLD） and diode array detector（DAD） to simultaneously analyze 16 polycyclic aromatic hydrocarbons（PAHs） in drinking water,including napthalene,acenaphtylene,acenaphthene,fluorene,phenanthrene,anthracene,fluoranthene,pyrene,benzo [a]anthracene,chrysene,benzo [b] fluoranthene,benzo [k]fluoranthene,benzo [a]pyrene,dibenz [a,h]anthracene,benzo [g,h,i]pyrene,indeo [1,2,3-cd]pyrene. Methods A total of 16 PAHs in 1 L drinking water were adsorbed by Bond Elut Plexa column and eluted with dichloromethane and ethyl acetate,the extracts were dried with nitrogen,diluted using 0.5 ml acetonitrile and filtered with 0.45 μm millipore filter. A total of 16 PAHs were chromatographically separated on a Pursuit PAHs column, the column temperature was 30 ℃, and gradiently eluted by the mobile phase composed of acetonitrile and aqueous solution, the flow rate was 1.8 ml/min. Acenaphthene was detected by DAD, while the other 15 PAHs were detected by FLD. Results The16 PAHs all had good relationships within the linear range of 0.000 5-100 mg/L（r〉0.998）. The limits of detection（LOD） were0.04-0.50 ng/L, the limits of quantification（LOQ） were 0.13-1.67 ng/L. The intra- and inter-day relative standard deviations（RSDs） of the mix standard solution were 1.0%-3.1% and 1.5%-3.8% respectively. Spiked recoveries of the analytes were77.7%-96.9% with RSDs 1.1%-4.2%. Conclusion The proposed method was rapid, accurate, sensitive and applicable to the simultaneously determination of 16 PAHs in drinking water.

关 键 词：水 色谱法 高效液相 荧光检测 二极管阵列检测 多环芳烃 

分 类 号：O657.6[理学—分析化学]