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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 establish a HPLC - FLD - DAD simultaneous determination method for 16 kinds of polycyclic aromatic hydrocarbons (PAHs) in drinking water. Methods 1 L water samples were adsorbed by Bond Elut Plexa solid phase extraction column and eluted with dichloromethane and ethyl acetate. After the eluate was purged with acetonitrile and then diluted to 0.5 ml with acetonitrile, the filtrate was filtered through 0.45 μm filter and purified with Pursuit PAHs column, the column temperature was 30 ℃. The mobile phase was eluted with acetonitrile-water as mobile phase with a flow rate of 1.8 ml / min. Fluorescence detection of naphthalene, acenaphthylene, phenanthrene, fluorene, anthracene, (A) pyrene, dibenzo [a, h] anthracene, benzo [g, h, i] perylene, Indeno [1,2,3-cd] pyrene 15 kinds of PAHs, DAD detection of camphene at 254 nm wavelength; injection volume 5.0μl. Results The regression equation of 16 PAHs showed good linearity (r> 0.998) within the linear range of 0.000 5 ~ 100 mg / L. The detection limit of this method was 0.04-0.50 ng / L, and the lower limit of quantification was 0.13-1.67 ng / L. The intra-day and inter-day RSD were 1.0% -3.1% and 1.5% -3.8%, respectively. The spiked recoveries were 77.7% ~ 96.9%, spiked RSD was 1.1% ~ 4.2%. Conclusion The method is rapid, accurate and sensitive and is suitable for the determination of 16 kinds of PAHs in drinking water.