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.
出处
《分析测试学报》
CAS
CSCD
北大核心
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)
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
benzotriazoles
benzothiazoles
solid-phase extraction
high performance liquid chro matography-tandem mass spectrometry（ HPLC -MS/MS）
surface water
