【摘要】 建立了水体中12种缓蚀剂(苯并噻唑和苯并三唑类衍生物)的大体积进样/气相色谱-质谱联用(PTV/GC-MS)的高灵敏度分析方法。1.0 L水样经0.45μm滤膜过滤后调至p H 3.0,通过HLB固相萃取柱富集。目标化合物经6 m L甲醇-乙腈(1∶1)淋洗,洗脱液用氮气吹扫至近干后,加入丙酮、内标物和硅烷化试剂定容至1 m L,置于烘箱中38℃衍生化1 h后,密封于细胞瓶中待测。试样采用DB-5MS气相色谱柱进行分离,选择离子模式(SIM)测定。结果表明,目标化合物在0.1~100 ng/L质量浓度范围内呈良好线性,相关系数均不小于0.992。自来水中12种化合物的平均加标回收率为46%~116%,相对标准偏差(RSD)为1.0%~16%。河水中目标化合物的回收率为43%~117%,RSD为1.0%~15%。自来水和河水中目标化合物的检出限分别为0.050~1.3 ng/L和0.057~1.8 ng/L。该方法成功用于广州珠江河段缓蚀剂污染物含量的分析。更多还原

【Abstract】 A rapid and reliable analytical method,based on large-volume injection and gas chromatography-mass spectrometry( PTV / GC-MS) was developed for the determination of 12 benzotriazoles and benzothiazoles in aquatic matrixes. 1. 0 L water samples were acidified to p H 3. 0 using 3mol / L HCl. The samples were then passed through an Oasis HLB cartridge. The analytes were eluted with 6 m L methanol-acetonitrile( 1 ∶ 1). The solution was evaporated to dryness under a gentle stream of nitrogen,and redissolved in acetone,internal standard and silylation reagent. The sealed vials were incubated at 38 ℃ for 1 h before instrument analysis. The separation of target compounds was achieved in a DB-5MS fused-silica capillary column. The analytes were detected in selected ion monitoring( SIM) that operated in electron impact( EI) mode. The calibration curves of 12 target compounds were linear in the range of 0. 1-100 ng / L with correlation coefficients not less than0. 992. Spiked recoveries of the target analytes were in the ranges of 46%-116% for tap water,and43%-117% for river water,with RSDs of 1. 0%-16% and 1. 0%-15%,respectively. The method detection limits for tap water and river water were in the ranges of 0. 050-1. 3 ng / L and 0. 057-1. 8 ng / L,respectively. The method was simple and sensitive,and was successfully employed in the detection of corrosion inhibitors in river water collected from the city section of the Pearl River.更多还原