固相萃取-高效液相色谱法测定地表水中的苯并三唑和苯并噻唑

Simultaneous determination of benzotriazoles and benzothiazole in surface water by solid phase extraction and high performance liquid chromatography

建立了固相萃取-高效液相色谱分析地表水中苯并噻唑、苯并三唑、5-甲基-苯并三唑、5-氯-苯并三唑及5,6-二甲基-苯并三唑的方法。地表水样品采用HLB固相萃取柱富集净化后,在甲醇-水(55∶45,v/v)流动相中用ZORB-AX SB-C18色谱柱(250 mm×4.6 mm,5μm)分离,紫外检测,外标法定量。结果表明,5种目标化合物在0.064～80 mg/L范围内均呈良好的线性关系,线性相关系数均大于0.999 9,仪器检出限为1.9～3.2μg/L。空白自来水样中的加标回收率为87.8%～125.6%,相对标准偏差(n=3)为0.4%～9.4%。应用该方法测定了大连自来水及辽河入海口水样,在辽河入海口地表水中检出苯并噻唑、苯并三唑、5-甲基-苯并三唑、5-氯-苯并三唑。

A simple method based on solid phase extraction （SPE） coupled with high performance liquid chromatography （HPLC） was developed for the determination of IH-benzotriazole （ BT ） , 5-methyl- l H-benzotriazole （ 5-M-BT）, 5,6-dimethyl- 1H-benzotriazole （ 5,6-DM-BT ） , 5- chloro-I H-benzotriazole （5-C1-BT） and benzothiazole （BTH） in surface water. The extraction and clean-up of the surface water sample were performed on an HLB solid-phase extraction car- tridge. The separation of the five compounds was achieved on a ZORBAX SB-CI8 column （250 mm ×4.6 mm, 5 μm） with methanol-water （55：45, v/v） as mobile phase and ultraviolet detection. The quantification was achieved by external standard method. The results showed that good linearities were observed in the ranges of 0. 064 - 80 mg/L with the correlation coeffi- cients≥ 0. 999 9 and the instrumental limits of detection for the five target compounds were in the range of 1.9 - 3.2 μg/L. The average recoveries of the five target compounds were 87.8% - 125.6% and the relative standard deviations （n = 3） were 0.4% -9.4%. This method was applied to the analysis of the surface water samples from the Dalian tap water and the Liaohe River estuary. The results showed that BT, 5-M-BT, 5-C1-BT and BTH were found in the water from the Liaohe River estuary.