固相萃取-大体积程序升温进样气相色谱-三重四极杆串联质谱测定饮用水中3种挥发性N-亚硝胺
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摘要
建立了固相萃取大体积程序升温进样气相色谱-三重四极杆质谱联用(GC-QqQ-MS/MS)同时测定饮用水中N-亚硝基二甲胺、N-亚硝基甲基乙基胺及N-亚硝基二乙基胺的分析方法。用椰壳活性炭固相萃取小柱萃取水样中待测物组分,少量二氯甲烷洗脱、无水硫酸钠脱水,大体积程序升温进样,气相色谱-三重四极杆质谱联用仪进行多反应监测(MRM)模式检测,外标法定量。3种N-亚硝胺在1～50 ng/L范围内线性关系良好,相关系数(r~2)均大于0.999,在饮用水中进行10、20和50 ng/L水平的添加,3种待测物平均加标回收率为94.8%～109%,相对标准偏差(RSD)为4.44%～8.10%(n=5),定量限(LOQ)为0.08～0.7 ng/L。该法灵敏、准确、简单、可靠,适用于饮用水中3种N-亚硝胺组分的痕量检测。
A method had been developed for the determination of three N-nitrosamines, namely, N-nitrosodimethylamine(NDMA), N-nitrosomethylethylamine(NMEA), and N-nitrosodiethylamine(NDEA) in drinking water by solid phase extraction(SPE) and gas chromatography-triple quadrupole mass spectrometry(GC-QqQ-MS/MS) with programmable temperature vaporizer(PTV)-based large volume injection(LVI). The N-nitrosamine compounds were extracted from the water sample using a solid phase extraction(SPE) cartridge filled with coconut charcoal, and then eluted with 10 mL methylene chloride. The eluate was dried by anhydrous sodium sulfate and 10 μL was injected into the GC-MS/MS by PTV-LVI. The target compounds were detected by the multi-reaction monitoring(MRM) mode, and quantified with the external standard method. The results showed that the three compounds had good linearities in the range of 1-50 ng/L with correlation coefficients(r~2) higher than 0.999. Drinking water samples were spiked with the target compounds at three concentration levels(10, 20, and 50 ng/L), and satisfactory recoveries(between 94.8% and 109%) and good reproductivities(relative standard deviation RSD<10%) were achieved. The limits of quantitation(LOQs) of the three N-nitrosamines were found to be in the range of 0.08-0.7 ng/L. The developed method was sensitive, accurate, convenient, and reliable for the determination of the three trace level N-nitrosamines in drinking water.
A method had been developed for the determination of three N-nitrosamines, namely, N-nitrosodimethylamine(NDMA), N-nitrosomethylethylamine(NMEA), and N-nitrosodiethylamine(NDEA) in drinking water by solid phase extraction(SPE) and gas chromatography-triple quadrupole mass spectrometry(GC-QqQ-MS/MS) with programmable temperature vaporizer(PTV)-based large volume injection(LVI). The N-nitrosamine compounds were extracted from the water sample using a solid phase extraction(SPE) cartridge filled with coconut charcoal, and then eluted with 10 mL methylene chloride. The eluate was dried by anhydrous sodium sulfate and 10 μL was injected into the GC-MS/MS by PTV-LVI. The target compounds were detected by the multi-reaction monitoring(MRM) mode, and quantified with the external standard method. The results showed that the three compounds had good linearities in the range of 1-50 ng/L with correlation coefficients(r~2) higher than 0.999. Drinking water samples were spiked with the target compounds at three concentration levels(10, 20, and 50 ng/L), and satisfactory recoveries(between 94.8% and 109%) and good reproductivities(relative standard deviation RSD<10%) were achieved. The limits of quantitation(LOQs) of the three N-nitrosamines were found to be in the range of 0.08-0.7 ng/L. The developed method was sensitive, accurate, convenient, and reliable for the determination of the three trace level N-nitrosamines in drinking water.
引文
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[3]Chen W W,Zhang Y,Li X S,et al.Chinese Journal of Environmental Chemistry,2016,35(10):2117陈文文,张原,李小水,等.环境化学,2016,35(10):2117
[4]Dong L,Wang H Y,Cai H Q,et al.Journal of Environment and Health,2016,33(3):232董蕾,王海燕,蔡宏铨,等.环境与健康杂志,2016,33(3):232
[5]International Agency for Research on Cancer.List of Classifications,Volumes 1-122.[2018-07-30].https://monographs.iarc.fr/list-of-classifications-volumes/
[6]Word Health Organization.Guidelines for Drinking-Water Quality.4th ed.Shanghai:Shanghai Jiao Tong University Press,2014世界卫生组织.饮用水水质准则.4版.上海:上海交通大学出版社,2014
[7]Luo Q,Wang D H,Wang B Y,et al.Scientia Sinica Chimica,2011,41(1):82罗茜,王东红,王炳一,等.中国科学:化学,2011,41(1):82
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[9]Zhao B,Deng M L,Yang X S,et al.Chinese Journal of Chromatography,2016,34(10):998赵博,邓美林,杨小珊,等.色谱,2016,34(10):998
[10]Yan Z Y,Niu Q Q,Mou M Y,et al.China Measurement&Test,2017,43(1):37严拯宇,牛倩倩,牟明瑶,等.中国测试,2017,43(1):37
[11]Yang H,Fang C F,Zhang T,et al.Chinese Journal of Food Research and Development,2016,37(3):150杨华,方长发,张甜,等.食品研究与开发,2016,37(3):150
[12]GB 5009.26-2016
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[16]Ma Q,Xi H W,Wang C,et al.Chinese Journal of Analytical Chemistry,2011,39(8):1201马强,席海为,王超,等.分析化学,2011,39(8):1201
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[18]Yu W J,Wang P,Qiu Y S,et al.Chinese Journal of Instrumental Analysis,2016,35(6):719余卫军,王佩,邱月生,等.分析测试学报,2016,35(6):719
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[21]Lu Y,Huang W,Fu N,et al.Chinese Journal of Gansu Science and Technology,2014,12(30):71陆荫,黄维,付宁,等.甘肃科技,2014,12(30):71
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[26]GB/T 5750.2-2006
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