卫生研究

目的建立高效液相色谱-紫外串联荧光检测器法同时检测水源水及自来水中的16种多环芳烃(polycyclic aromatic hydrocarbons,PAHs)。方法水源水样品预先经GF/C玻璃纤维滤纸过滤,自来水样品采样时即按每升水加入60 mg抗坏血酸消除余氯干扰。取500 mL水样,磷酸调节pH至2,加入10 mL甲醇,混匀。样品经苯乙烯二苯乙烯聚合物柱富集,50%甲醇(pH 2)润洗样品瓶后继续上样,80%甲醇去除杂质,二氯甲烷洗脱。洗脱液加入100μL 10%吐温-20甲醇溶液(m/V)后氮吹至近干,乙腈复溶,经PAH液相色谱柱(250 mm×4.6 mm,5μm)在乙腈和水为流动相下梯度分离,紫外检测器串联荧光检测器检测,外标法定量。结果 16种PAHs在0.5～500 ng/mL范围内线性关系良好,相关系数均大于0.999;方法的检出限为0.3～5 ng/L,定量限为1.2～20 ng/L,回收率为67.2%～114.1%,相对标准偏差为1.5%～14.0%(n=6)。采用该方法对17份实际样品进行检测,在水源水、出厂水和末梢水中分别检测到8种、6种和7种目标化合物。结论该方法操作简单、灵敏度高、选择性好,适用于水源水和自来水中16种PAHs的检测。

OBJECTIVE To establish a rapid method for simultaneous determination of 16 polycyclic aromatic hydrocarbons(PAHs) in source water and tap water by performance liquid chromatography(HPLC) with ultraviolet detector(UV) tandem fluorescence detector(FLR). METHODS Source water was filtered by GF/C glass fiber filters and tap water were added ascorbic acid of 60 mg per liter to remove the residual chlorine when sampling. 500 mL water sample were sampled and adjusted pH 2 with phosphoric acid, then 10 mL methanol were added. Then samples were concentrated by styrene stilbene polymer solid phase extraction column, after loading samples, 50 percent methanol aqueous solution adjust pH 2 were used for washing bottle and the washed solution were continuum loaded. Then 80 percent methanol aqueous solution was used for removing impurity interference and elution with dichloromethane. The eluent was nitrogen blow to near dry after adding 100 μL 10 percent tween-20 methanol solutions(m/V). Acetonitrile was used for reconstitution, and then separated by PAH chromatography column using acetonitrile and pure water at gradient elution, and detected by UV tandem FLR detector. RESULTS The linear ranges of 16 PAHs were 0.5 to 500 ng/mL and the correlation coefficients were greater than 0.999. The method detection limit and limits of quantification were 0.3 to 5.0 ng/L and 1.2 to 20.0 ng/L, respectively. The recoveries were in the range of 67.2%-114.1% with the relative standard deviations ranging from 1.5%-14.0%(n=6). Then the established method was used for the determination of 17 water samples, 8 kinds, 6 kinds and 7 kinds of PAHs were detected in source water, tap water and pipe net tap water, respectively. CONCLUSION The method is rapid, sensitive and selective, and has been successfully applied for determination of 16 PAHs in source water and tap water.