超高效液相色谱-串联四级杆/飞行时间质谱法在饮用水检测中的应用
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摘要
目的应用超高效液相色谱-串联四级杆/飞行时间质谱结合二元比较的方法,对2种水样品进行检测研究,建立辨别饮用水质量的检测方法。方法样品经Oasis HLB固相萃取柱和滤膜过滤处理后,用含有10mmol/L乙酸铵的水溶液和含有10 mmol/L乙酸铵的甲醇溶液进行洗脱,再经超高效液相色谱分离后进入四级杆飞行时间质谱,实验通过保留时间、精确质量数、质量偏差等参数进行定性研究。结果通过二元比较找出2种水之间的差异,并鉴定出百治磷、阿特拉津、脱乙基阿特拉津、环嗪酮、莠谷隆、另丁津、邻苯二甲酸丁苄酯、噻嗪酮等8种污染物。结论此方法不仅能够直观地辨别出2种水样品的差异,而且可以准确鉴定差异化合物,适用于饮用水的检测研究。
Objective To establish a detection method for distinguish the quality of drinking water through detecting the two kinds of water samples by ultra performance liquid chromatography tandem quadrupole-time of flight mass spectrometry(UPLC-QTOF-MS). Methods The pretreatments of water samples were conducted by Oasis HLB solid phase extraction column and organic filter. Then sample solvent was diluted with water(with 10 mmol/L ammonium acetate) and methanol(with 10 mmol/L ammonium acetate). The eluent from the UPLC was further detected by QTOF-MS. The retention time, exact mass and mass error were used to qualify the compounds screened in this study. Results Differences between the two kinds of water were characterized by binary comparison, and 8 kinds of pollutants were identified, including dicrotophos, atrazine, atrazine-desethyl, hexazinone, metobromuron, sebuthylazine, benzyl butyl phthalate and buprofezin. Conclusion The established method not only can distinguish the differences between the two kinds of water samples, but also can accurately identify the different compounds, which is suitable for the detection of drinking water.
Objective To establish a detection method for distinguish the quality of drinking water through detecting the two kinds of water samples by ultra performance liquid chromatography tandem quadrupole-time of flight mass spectrometry(UPLC-QTOF-MS). Methods The pretreatments of water samples were conducted by Oasis HLB solid phase extraction column and organic filter. Then sample solvent was diluted with water(with 10 mmol/L ammonium acetate) and methanol(with 10 mmol/L ammonium acetate). The eluent from the UPLC was further detected by QTOF-MS. The retention time, exact mass and mass error were used to qualify the compounds screened in this study. Results Differences between the two kinds of water were characterized by binary comparison, and 8 kinds of pollutants were identified, including dicrotophos, atrazine, atrazine-desethyl, hexazinone, metobromuron, sebuthylazine, benzyl butyl phthalate and buprofezin. Conclusion The established method not only can distinguish the differences between the two kinds of water samples, but also can accurately identify the different compounds, which is suitable for the detection of drinking water.
引文
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[15]霍丽娟.阿特拉津及其两种代谢产物在砂质壤土中吸附、降解和淋溶规律的实验研究[D].北京:中国农业大学,2006.Huo LJ.Experimental study on adsorption,degradation and leaching of atrazine and its metabolites in sandy loamy soil[D].Beijing:China Agriculture University,2006.
[2]于建,査玉娥,卞战强,等.我国南北典型省份农村饮用水中农药残留的现状调查[J].环境与健康杂志,2015,32(8):721?723.Yu J,Cha YE,Bian ZQ,et al.Investigation on pesticides residues in rural drinking water in typical provinces of north and south China[J].J Environ Health,2015,32(8):721?723.
[3]黄士新,李丹妮,张文刚,等.畜禽场周边土壤和水中环丙氨嗪和三聚氰胺污染情况调查[J].农业资源与环境学报,2010,27(2):87?90.Huang SX,Li DN,Zhang WG,et al.Investigation on the pollution of cyclamazine and melamine in the soil and water around livestock and poultry farm[J].Agro-Environ Dev,2010,27(2):87?90.
[4]胡春华,周文斌,黄宗兰,等.环鄱阳湖区农村饮用水重金属健康风险评价[J].江西师范大学学报:自然科学版,2010,34(1):102?106.Hu CH,Zhou WB,Huang ZL,et al.Health risk assessment of heavy metals in rural drinking waters around the district of poyang lake[J].J Jiangxi Norm Univ:Nat Sci Ed,2010,34(1):102?106.
[5]杨晓芬,赵美萍,李元宗,等.水中苯胺类化合物的分光光度法测定[J].分析化学,2002,30(5):540?543.Yang XF,Zhao MP,Li YZ,et al.Spectrophotometric methods for the determination of aniline in water[J].Chin J Anal Chem,2002,30(5):540?543.
[6]刘勇建,牟世芬,林爱武,等.大体积直接进样离子色谱法测定饮用水中9种卤代乙酸和6种阴离子[J].色谱,2003,21(2):181?183.Liu YJ,MU SF,Lin AW,et al.Determination of nine haloacetic acids and six anions in drinking water by ion chromatography with large volume direct injection[J].Chin J Chromatogr,2003,21(2):181?183.
[7]王坚民.水中环丁砜气相色谱测定法研究[J].预防医学情报杂志,2005,21(6):749?751.Wang JM.Experiment study on detection of sulfolane in water by gas chromatography[J].J Pre Med Inf,2005,21(6):749?751.
[8]李彦文,莫测辉,赵娜,等.高效液相色谱法测定水和土壤中磺胺类抗生素[J].分析化学,2008,36(7):954?958.Li YW,MO CH,Zhao N,et al.Determination of sulfonamides antibiotics in water and soil using high performance liquid chromatography[J].Chin J Anal Chem,2008,36(7):954?958.
[9]俞博凡,温丽丽,宋永会,等.膜进样/飞行时间质谱实时分析水源水中挥发性有机污染物[J].光谱学与光谱分析,2011,31(8):2259?2262.Yu BF,Wen LL,Song YH,et al.Realtime analysis of volatile organic compounds in source water by membrane inlet/time-of-flight mass spectrometry[J].Spectrosc Spectr Anal,2011,31(8):2259?2262.
[10]尹燕敏,沈颖青,顾海东,等.固相萃取-液质联用法同时测定水中的喹诺酮类和磺胺类抗生素[J].化学分析计量,2013,(3):29?32.Yin YM,Shen YQ,Gu HD,et al.Simultaneous determination of quinolones and sulfonamides in water samples by solid phase extract ion-ultra performance liquid chromatography electrospray tandem mass spectrometry[J].Chem Anal Meter,2013,(3):29?32.
[11]张晓波,黄丽英,陈万勤,等.应用飞行时间质谱测定食品中多种真菌毒素的研究进展[J].浙江农业科学,2013,(7):849?852.Zhang XB,Huang LY,Chen WQ,et al.Advances in determination of mycotoxins by time-of-flight mass spectrometry in foods[J].J Zhejiang Agric Sci,2013,(7):849?852.
[12]权彦.薄层扫描法检测益母草中农药百治磷的限量[J].陕西中医学院学报,2007,30(3):47.Quan Y.Determination of the pesticide limit of leonurus japonicus by TLC scanning[J].J Shaanxi Coll Tradit Chin Med,2007,30(3):47.
[13]谢梦醒,李学德,花日茂,等.高效液相色谱法测定甘蔗及土壤中环嗪酮的残留量[J].农药学学报,2011,13(1):95?98.Xie MX,Li XD,Hua RM,et al.Determination of hexazinone residues in sugarcane and soil by high performance liquid chromatography[J].Chin J Pest Sci,2011,13(1):95?98.
[14]张璐璐,刘静玲,何建宗,等.中国典型城市水环境中邻苯二甲酸酯类污染水平与生态风险评价[J].生态毒理学报,2016,11(2):421?435.Zhang LL,Liu JL,He JZ,et al.The occurrence and ecological risk assessment of phthalate esters(PAEs)in urban aquatic environments of China[J].Asian J Ecotoxicol,2016,11(2):421?435.
[15]霍丽娟.阿特拉津及其两种代谢产物在砂质壤土中吸附、降解和淋溶规律的实验研究[D].北京:中国农业大学,2006.Huo LJ.Experimental study on adsorption,degradation and leaching of atrazine and its metabolites in sandy loamy soil[D].Beijing:China Agriculture University,2006.