全自动固相萃取-气相色谱-串联质谱法测定生活饮用水中5种亚硝胺
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摘要
目的建立一种适合同时测定生活饮用水中5种亚硝胺的气相色谱-串联质谱检测方法。方法采用Cleanert pesticarb固相萃取柱对样品进行前处理,DB-35MS毛细管柱(30 m×0.25 mm,0.25μm)进行分离,单离子监测扫描模式(SIM)扫描,并对离子效应、pH值和洗脱液流速进行优化,建立了全自动固相萃取-气相色谱-串联质谱测定生活饮用水中5种亚硝胺的方法。结果 5种亚硝胺在0.05～1.00μg/L范围内线性良好,N-亚硝基-二甲胺、N-亚硝基-二乙胺、N-亚硝基-二丙胺、N-亚硝基-二丁胺和N-亚硝基-二苯胺的检出限分别为0.001、0.001、0.000 5、0.02和0.002μg/L(信噪比=3)。在优化条件下,对实际水样进行低、中、高3个不同浓度的加标试验,回收率在70.32%～96.39%范围内,相对标准偏差为2.98%～5.29%(n=6)。结论该方法灵敏度高、线性范围广,优化了生活饮用水中5种亚硝胺的检测条件,适用于生活饮用水中亚硝胺的检测。
Objective An analytical method for determination of five N-nitrosoamine in water samples was developed using solid-phase extraction and gas chromatography/mass spectrometry(SPE-GC-MS/MS). Methods The samples were pretreated with Cleanert pesticarb SPE solid phase extraction column, then separated by DB-35 MS(30 m×0.25 mm,0.25 μm) chromatographic column under, select ion scanning mode(SIM). The determination of five N-nitrosoamine in drinking water by gas chromatography-mass spectrometry method was established by the optimization of ion effect, pH and eluent flow rate. Results The result showed that all five N-nitrosoamine had good linearities in the range of 0.05 to 1.00 μg/ml,the detection limits for 5 nitrosamines were 0.001,0.001,0.000 5,0.02 and 0.002 μg/L(S/N=3). The average recovery rates measured by standard addition method were in the range of 70.32%-96.39% with the relative standard deviation(n=6) in the range of 2.98%-5.29%. Conclusion The method had high sensitivity, wide linear range and optimized the detection conditions of five N-nitrosoamine in drinking water, and it was suitable for the detection of N-nitrosodamine in drinking water.
Objective An analytical method for determination of five N-nitrosoamine in water samples was developed using solid-phase extraction and gas chromatography/mass spectrometry(SPE-GC-MS/MS). Methods The samples were pretreated with Cleanert pesticarb SPE solid phase extraction column, then separated by DB-35 MS(30 m×0.25 mm,0.25 μm) chromatographic column under, select ion scanning mode(SIM). The determination of five N-nitrosoamine in drinking water by gas chromatography-mass spectrometry method was established by the optimization of ion effect, pH and eluent flow rate. Results The result showed that all five N-nitrosoamine had good linearities in the range of 0.05 to 1.00 μg/ml,the detection limits for 5 nitrosamines were 0.001,0.001,0.000 5,0.02 and 0.002 μg/L(S/N=3). The average recovery rates measured by standard addition method were in the range of 70.32%-96.39% with the relative standard deviation(n=6) in the range of 2.98%-5.29%. Conclusion The method had high sensitivity, wide linear range and optimized the detection conditions of five N-nitrosoamine in drinking water, and it was suitable for the detection of N-nitrosodamine in drinking water.
引文
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[10] FUJIOKA T, TAKEUCHI H, TANAKA H, et al. Arapid and riliable technique for N-nitrosodimethylamine analysis in reclaimed water by HPLC-photochemical reaction-chemilumin-escenci[J]. Chemosphere, 2016,161(6):104-111.
[11] 陈忠林,徐冰冰,齐虹,等.高效液相色谱测定水中痕量亚硝基二甲胺[J].中国给水排水,2007,23(8):84-87.
[12] PLUMLEE M H, LóPEZ-MESAS M, HEIDLBERGER A, et al. N-nitrosodimethylamine (NDMA) removal by reverse osmosis and UV treatment and analysis via LC-MS/MS[J].Water Res,2008,42 (1/2): 347-355.
[13] KADMI Y, FAVIER L, SIMION A I, et al. A rapid and sensitive method for the monitoring of N-nitrosodiphenylamine and N-nitrosodimethylamine in multiple water matrices[J].Carpath J Earth Env,2015,10(1): 53-61.
[14] WANG W F, HU J Y, YU J W, et al. Determination of N-nitrosodimethylamine in drinking water by UPLC-MS/MS[J]. Journal of Environmental Sciences, 2010,22(10):1508-1512.
[15] 朱翔,李伟,刘玉灿,等.超高效液相色谱-三重四级杆质谱联用仪同时检测水中9种亚硝胺[J].分析测试学报,2014,33(8):866-871.
[2] MCDONALD J A, HARDEN N B, NGHIEM L D, et al. Analysis of N-nitrosamines in water by isotope dilution gas chromatography-electron ionisation tandem mass spectrometry [J].Talanta,2012,99(5):146-154.
[3] CHOI J,VALENTINE R L.Formation of N-nitrosodimethylamine(NDMA)from reaction of monochloramine:a new disinfection by-product[J].Water Res,2002,36(4),817-824.
[4] ASAMI M, OUA M, KOSAKA K. A nationwide survey of NDMA in raw and drinking water in Japan[J].Sci Total Environ, 2009,407(11):3540-3545.
[5] KADMI Y, FAVIER L, SOUTREL I, et al. Ultratrace-level determination of N-nitrosodimethylamine, N-nitrosodiethylamine, and N-nitrosomorpholine in water by solid-phase extraction followed by liquid chromatography-tandem mass spectrometry[J].Central European Journal of Chemistry, 2014,12(9):928-936.
[6] ANDRZEJEWSKI P, KASPRZYK-HORDEN B, NAWROCKI J. N-nitrosodimethylamine(NDMA) formation during ozonation of dimethylamine-containing waters[J].Water Res, 2008, 42(4/5):863-870.
[7] JURADO-SANCHEZ B, BALLESTEROS E, GALLEGO M, et al. Fullerenes for aromatic and non-aromatic nitrosamines discrimination[J]. Journal of Chromatogr A, 2009, 1216(7): 1200-1205.
[8] GREBEK J E,YOUNG C C, SUFFET I H. Solid-phase microextraction of N-nitrosamines[J]. Journal of Chromatogr A,2006,1117(1):11-18.
[9] 刘清明,张雪晨,周全,等.一种基于气相色谱-质谱检测水质N-亚甲基二甲胺(NDMA)的固相萃取方法[J].环境化学, 2011,3(7):1327-1331.
[10] FUJIOKA T, TAKEUCHI H, TANAKA H, et al. Arapid and riliable technique for N-nitrosodimethylamine analysis in reclaimed water by HPLC-photochemical reaction-chemilumin-escenci[J]. Chemosphere, 2016,161(6):104-111.
[11] 陈忠林,徐冰冰,齐虹,等.高效液相色谱测定水中痕量亚硝基二甲胺[J].中国给水排水,2007,23(8):84-87.
[12] PLUMLEE M H, LóPEZ-MESAS M, HEIDLBERGER A, et al. N-nitrosodimethylamine (NDMA) removal by reverse osmosis and UV treatment and analysis via LC-MS/MS[J].Water Res,2008,42 (1/2): 347-355.
[13] KADMI Y, FAVIER L, SIMION A I, et al. A rapid and sensitive method for the monitoring of N-nitrosodiphenylamine and N-nitrosodimethylamine in multiple water matrices[J].Carpath J Earth Env,2015,10(1): 53-61.
[14] WANG W F, HU J Y, YU J W, et al. Determination of N-nitrosodimethylamine in drinking water by UPLC-MS/MS[J]. Journal of Environmental Sciences, 2010,22(10):1508-1512.
[15] 朱翔,李伟,刘玉灿,等.超高效液相色谱-三重四级杆质谱联用仪同时检测水中9种亚硝胺[J].分析测试学报,2014,33(8):866-871.