固相萃取高效液相色谱-串联质谱法测定地表水中苯并三唑类及苯并噻唑类衍生物  

Simultaneous Determination of Benzotriazoles and Benzothiazoles in Surface Water by Solid Phase Extraction and High Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：王金成[1] 张海军[1] 陈吉平[1] 

机构地区：[1]中国科学院大连化学物理研究所,辽宁大连116023

出　　处：《分析测试学报》2013年第9期1056-1061,共6页Journal of Instrumental Analysis

基　　金：国家"973计划"项目(2009CB421602);国家自然科学基金项目(21277139)

摘　　要：建立了环境水样中8种苯并三唑类和苯并噻唑类化合物：苯并三唑（1H-benzotriazole,BTri）、5-甲基苯并三唑（5-Methyl-1H-benzotriazole,5-TTri）、5,6-二甲基苯并三唑（5,6-Dimethyl-1H-benzotriazole,5,6-DMBTri）、5-氯-苯并三唑（5-Chloro-1H-benzotriazole,5-ClBTri）、1-羟基苯并三唑（1-Hydroxybenzotriazole,1-OHBTri）、苯并噻唑（Benzothiazole,BT）、2-氨基苯并噻唑（2-Aminobenzothiazole,2-ABT）和2-甲基苯并噻唑（2- Methylbenzothiazole,2-TBT）的高效液相色谱-串联质谱（LC-MS/MS）分析方法。200 mL 环境水样经 0.22 μm 滤膜过滤后用盐酸（1∶1）调至 pH 3.0,过 HLB 固相萃取柱,经3 mL 10% 甲醇水溶液淋洗,6 mL丙酮-甲醇（2∶8,体积比）洗脱。目标化合物经Hypersil GOLD型色谱柱（150 mm×2.1 mm）结合甲醇-水-乙腈梯度洗脱分离后,用正离子多重反应监测模式进行质谱分析。结果表明,1.OHBTri、BT及2-TBT的线性范围为8-1 000 μg/L,其他5种化合物的线性范围为1.6-1 000 μg/L,相关系数均大于0.99。8 种化合物的基质加标回收率为 59.8%-98.7%,相对标准偏差（n=5）为 0.9%-12.5%,方法的检出限（S/N=3）为 0.03-1.4 μg/L。A simple method based on SPE coupled with HPLC-MS/MS was developed for the determination of 1H-benzotriazole（BTri）,5-methyl-1H-benzotriazole（5-TTri）,5,6-dimethyl-1H-benzotriazole（5,6-DMBTri）,5-chloro-1H-benzotriazole（5-ClBTri）,1-hydroxybenzotriazole（1-OHBTri）,benzothiazole（BT）,2-aminobenzothiazole（2-ABT） and 2-methylbenzothiazole（2-TBT） in surface water.Extraction and cleanup of surface water samples were performed on an HLB solid-phase extraction cartridge.The optimum extraction process was as follows：pH value of sample：3.0,sampling volume：200 mL,washing solvent：3 mL 10% methanol,eluting solvent：6 mL 20% acetone in methanol.Separation of target compounds was achieved on a Hypersil GOLD analytical column（150 mm×2.1 mm） with methanol-acetonitrile-water as mobile phase by gradient elution.Quantitative analysis by ESI-MS/MS was achieved using positive ion mode with multiple reaction monitoring mode.The calibration curves were linear in the range of 8-1 000 μg/L for 1-OHBTri,BT and 2-TBT,and 1.6-1 000 μg/L for rest of the compounds,with correlation coefficients more than 0.99.The average recoveries of target compounds were in the range of 59.8%-98.7% with relative standard deviations（RSDs,n=5） of 0.9%-12.5%.The instrumental limits of detection（S/N=3） for eight target compounds were in the range of 0.03-1.4 μg/L.

关 键 词：苯并三唑衍生物 苯并噻唑衍生物 固相萃取 高效液相色谱串联质谱 地表水 

分 类 号：O657.63[理学—分析化学] TQ072[理学—化学]