水中9种亚硝胺类化合物的固相萃取-气相色谱质谱联用测定方法  

Determination of nine nitrosamines in water by solid phase extraction and gas chromatography-mass spectrometry

作　　者：沈朝烨[1] 蔡宏铨 裴赛峰[1] 张昀[1] SHEN Chao-ye;CAI Hong-quan;PEI Sai-feng;ZHANG Yun(Division of Chemical Toxicity and Safety Assessment,Shanghai Municipal Center for Disease Control and Prevention,Shanghai 200336,China)

机构地区：[1]上海市疾病预防控制中心化学品毒性检定所

出　　处：《环境与职业医学》2019年第11期1060-1065,共6页Journal of Environmental and Occupational Medicine

摘　　要：[背景]亚硝胺类化合物(NAms)是一类新型消毒副产物,其种类较多、毒性较大,对人群健康具有潜在危害。目前,国内饮用水监测领域未颁布相关标准方法。[目的]建立优化同时测定生活饮用水及其水源水中9种NAms的固相萃取-气相色谱-质谱法。[方法]500 mL水样通过椰壳炭填料固相萃取小柱进行NAms富集,二氯甲烷洗脱,同位素内标加入法定量,使用VF-624 MS色谱柱,气相色谱-质谱联用检测。采集上海不同类型水样以检测NAms含量。[结果]NAms待测物在10~500 ng/L范围内线性良好,相关系数均大于0.995,分别以纯水和水源水为基质,方法检出限均低于4 ng/L。加标浓度为20、100、200 ng/L时,纯水、水源水和管网水中NAms的加标回收率在68.7%~113%之间,相对标准偏差均在10%以下。上海不同类型水样均可检出NAms,其中N-二甲基亚硝基胺(NDMA)和N-二正丁基亚硝基胺(NDBA)检出率最高。[结论]本方法灵敏度高、检出限低、准确度好,可实现水中9种NAms的同时测定。[Background] Nitrosamines in drinking water are a new group of disinfection by-products, with various kinds, high toxicity, and potential health hazards. At present, no relevant standards and methods are issued in the field of drinking water monitoring in China. [Objective] This methodological study aims to develop and modify a solid phase extraction(SPE) and gas chromatography-mass spectrometry(GC-MS) for the simultaneous determination of nine nitrosamines in drinking water and source water.[Methods] Nitrosamines were extracted by passing a 500 mL water sample through a SPE cartridge composed of coconut charcoal. After elution with methylene chloride, the extracts were analyzed by GC-MS with a VF-624 MS column using isotope internal standard. Nitrosamines in different kinds of water samples collected in Shanghai were detected by the established method.[Results] The calibration curves of nitrosamines had good linearity in 10-500 ng/L with correlation coefficients greater than 0.995. The method detection limits for both pure water and source water were below 4 ng/L. Recoveries ranged between 68.7%-113% with the relative standard deviations below 10% at 20, 100, and 200 ng/L for pure water, source water, and pipe water, respectively. Nitrosamines were detected in various water samples from Shanghai, with highest positive rates of N-nitrosodimethylamine(NDMA) and N-nitrosodibutylamine(NDBA).[Conclusion] This method featured with high sensitivity, low detection limit, and good accuracy is applicable to the determination of nine nitrosamines in water simultaneously.

关 键 词：气相色谱-质谱法 固相萃取 亚硝胺 椰壳炭 生活饮用水 水源水 

分 类 号：R115[医药卫生—公共卫生与预防医学]