固相萃取-气相色谱-串联质谱法测定水中15种N-亚硝胺类化合物  

Analysis of 15 nitrosamine compounds in water by solid phase extraction-gas chromatography-tandem mass spectrometry

作　　者：林华影[1] 林捷[1] 张伟[1] 林侃[1] 陈敏红[1] 张秋[1] LIN Hua-ying;LIN Jie;ZHANG Wei;LIN Kan;CHEN Min-hong;ZHANG Qiu(Puzhou Municipal Center for Disease Control and Prevention,Fuzhou,Fujian 350004,China)

机构地区：[1]福建省福州市疾病预防控制中心,福建福州350004

出　　处：《中国卫生检验杂志》2022年第8期908-913,共6页Chinese Journal of Health Laboratory Technology

基　　金：福州市科技计划项目(2019-SZ-65)。

摘　　要：目的建立同时测定水中15种N-亚硝胺类化合物的固相萃取-气相色谱-串联质谱法。方法用椰壳活性炭固相萃取小柱提取水样中的N-亚硝胺类化合物,以乙酸乙酯、二氯甲烷洗脱,氮吹浓缩定容,用HP-INNOWax毛细管柱色谱分离,三重四级杆气相色谱-串联质谱多反应监测模式(MRM)检测,内标法定量。结果方法相对标准偏差<4.02%,各组分标准曲线的相关系数>0.9981,检出限为0.24 ng/L~0.52 ng/L,3个浓度水平的加标回收率为86.1%~104.7%。结论该方法各项指标满足痕量物质检测分析要求,前处理快速简捷,易于操作。同时,该方法选择性好,灵敏度和准确性高,化学背景低,对水样适应性好,适合于水中15种N-亚硝胺类化合物的同时检测,可为我国建立水质样品中亚硝胺类化合物的标准检测方法提供借鉴和参考。Objective To develop a method for the simultaneous detection of 15 nitrosamine compounds in water by solid phase extraction-gas chromatography-tandem mass spectrometry. Methods The target analytes in water samples were extracted with coconut shell-activated carbon solid phase column and eluted with ethyl acetate,dichloromethane,then separated with a HP-INNOWax capillary column. The detection was accomplished with triple quadrupole mass spectrometry( Qq Q-MS/MS)and the quantification was based on internal standard curves. Results The correlation coefficients of the method were greater than 0. 998 1,with relative standard deviations( RSDs) less than 4. 02%. The limits of quantification were within 0. 24 ng/L-0. 52 ng/L,and the recoveries determined at three spiked levels were within 86. 1%-104. 7%. Conclusion The indicators of this method achieved the requirement that the detection and analysis of trace substances. This proposed method is rapid and convenient for the determination,and easy for the operation. This method is selective,sensitive and accurate. It has low chemical background and good adaptability to water samples. This method is suitable for simultaneous determination of 15 nitrosamine compounds in water. This method can provide a reference for the detection of nitrosamine compounds in water samples and for the establishment of standard detection method.

关 键 词：N-亚硝胺类化合物 水 固相萃取法 气相色谱-串联质谱法 

分 类 号：O657[理学—分析化学]