全自动固相萃取-气相色谱-串联质谱法测定水质中N-亚硝胺类化合物  

Determination of nine N-nitrosamines in water by gas chromatography- tandem mass spectrometry with auto-solid phase extraction

作　　者：何书海[1,2] 曹小聪[1,2] 李腾崖 张鸣珊[1,2] 梁焱[1,2] 陈表娟 庄健[1,2] HE Shuhai;CAO Xiaocong;LI Tengya;ZHANG Mingshan;LIAN Yan;CHEN Biaojuan;ZHUANG Jian(Hainan Province Research Academy of Environmental Sciences Haikou, 570206, China;Hainan Province Environmental Monitoring Centre, Haikou, 570206, China)

机构地区：[1]海南省环境科学研究院,海口570206 [2]海南省环境监测中心站,海口570206

出　　处：《环境化学》2019年第5期1197-1200,共4页Environmental Chemistry

摘　　要：本文采用全自动固相萃取-气相色谱-串联质谱(GC-MS/MS)分析水质中9种N-亚硝胺类化合物.水样以10 mL·min^-1速度通过Cleanert NDMA-SPE(1000 mg/6 mL)进行富集,用20%的甲醇水溶液淋洗去除杂质和破坏柱填料表层的水膜,再用二氯甲烷溶剂洗脱,收集的固相萃取洗脱液浓缩后进行GC-MS/MS分析.采用Rtx-Wax色谱柱分离,MRM模式下进行检测,内标法定量.实验结果表明,9种目标物在1.00-100μg·L^-1范围内线性关系良好,相关系数大于0.999;方法检出限为0.1-0.5 ng·L^-1.在低、中、高的加标水平下,9种N-亚硝胺类化合物的回收率分别为71%-94%、74%-95%和75%-103%,相对偏差分别为6.7%-15.8%、5.1%-12.3%和4.5%-9.6%.In this study, a method for the determination of nine N-nitrosamines in water was established by auto-solid phase extraction(ASPE)-gas chromatography-tandem mass spectrometry(GC-MS/MS). After the water samples were enriched by NDMA-SPE at a speed of 10 mL·min-1, the impurities and the water film on the surface of SPE bed were removed by leaching with 20% methanol water solution. The analytes were eluted and collected from the SPE bed with dichloromethane. After concentration, the quantitative analysis was conducted through GC-MS/MS. The analytes were separated on a Rtx-Wax chromatographic column,and ionized by electron impact(EI) source. The data were collected by multiple reaction monitoring(MRM) mode,followed by quantitative analysis using internal standard method. The correlation coefficients of linear calibration curves were over 0.999 in the corresponding linear ranges(1.00-100 μg·L^-1). The method detection limit was 0.1-0.5 ng·L^-1. The recovery rates of the nine N-nitrosamine compounds were 71%-94%, 74%-95% and 75%-103% at the low, medium and high spike levels, respectively. The corresponding relative deviations were 6.7%- 15.8%, 5.1%- 12.3% and 4.5%- 9.6%, respectively.

关 键 词：固相萃取 气相色谱-串联质谱 亚硝胺类化合物 水质 

分 类 号：O657.63[理学—分析化学] X832[理学—化学]