GC和HPLC测定水质中丙烯酰胺的比较
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摘要
分别建立了气相色谱法和液相色谱法测定水质中丙烯酰胺的分析方法,并比较2种方法的优缺点。GC法是丙烯酰胺在酸性条件下经溴化衍生后,再用乙酸乙酯萃取,然后经佛罗里硅土柱净化,最后利用气相色谱仪-电子捕获检测器分析。该方法的检出限为0.07μg/L,线性范围为0.50～12.5μg/L,加标回收率为82.0%～92.8%,相对标准偏差为3.4%～6.9%。HPLC法是水样经过滤后通过活化后ACA丙烯酰胺专用柱,用甲醇洗脱,最后利用液相色谱仪-紫外检测器分析。该方法的检出限为0.05μg/L,线性范围为0.10～2.00mg/L,加标回收率为85.0%～94.5%,相对标准偏差为2.6%～6.3%。综合比较2种方法,液相色谱法更适合于水质中丙烯酰胺的准确定性与定量分析,前处理更简便、快速,检出限更低,平均加标回收率更高,相对标准偏差更小,方法稳定性更高。
In this paper, two methods were developed for the detection of Acrylamide in water by using gas chromatography(GC) and high performance liquid chromatography(HPLC), and the advantages and disadvantages of the two methods were compared. The GC method: Acrylamide was extracted by ethyl acetate after bromide derivatization under acidic conditions, then purified by florid silica column, and finally analyzed by gas chromatography-electron capture detector. The detection limit of GC method was 0.07μg/L, the linear range was 0.50～12.5μg/L, the recovery was 82.0%～92.8%, and the relative standard deviation(RSD) was 3.4%～6.9%. The steps of HPLC method are as follows: the filtered water sample was passed through the activated ACA acrylamide column, then the column was eluted by methanol, and finally the extracts were analyzed by liquid chromatography-UV detector. The detection limit of HPLC method was 0.05μg/L, the linear range was 0.10～2.00 mg/L, the recovery was 85.0%～94.5%, and the relative standard deviation was 2.6%～6.3%. Through comprehensive comparison of the two methods, it can be found that HPLC was more suitable for accurate qualitative and quantitative analysis of acrylamide in water in term of simplicity, speed, detection limit, precision and stability.
In this paper, two methods were developed for the detection of Acrylamide in water by using gas chromatography(GC) and high performance liquid chromatography(HPLC), and the advantages and disadvantages of the two methods were compared. The GC method: Acrylamide was extracted by ethyl acetate after bromide derivatization under acidic conditions, then purified by florid silica column, and finally analyzed by gas chromatography-electron capture detector. The detection limit of GC method was 0.07μg/L, the linear range was 0.50～12.5μg/L, the recovery was 82.0%～92.8%, and the relative standard deviation(RSD) was 3.4%～6.9%. The steps of HPLC method are as follows: the filtered water sample was passed through the activated ACA acrylamide column, then the column was eluted by methanol, and finally the extracts were analyzed by liquid chromatography-UV detector. The detection limit of HPLC method was 0.05μg/L, the linear range was 0.10～2.00 mg/L, the recovery was 85.0%～94.5%, and the relative standard deviation was 2.6%～6.3%. Through comprehensive comparison of the two methods, it can be found that HPLC was more suitable for accurate qualitative and quantitative analysis of acrylamide in water in term of simplicity, speed, detection limit, precision and stability.
引文
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[4]国家环境保护总局,国家质量监督检验检疫总局.GB3838-2002.地表水环境质量标准[S].北京:中国环境科学出版社,2002.
[5]田好亮.毛细管柱气相色谱法测定水中丙烯酰胺[J].环境卫生学杂志,2013,03(05):455-457.
[6]张凤菊,金玲仁,李红莉.溴化衍生-气相色谱法测定地表水中丙烯酰胺[J].中国环境管理干部学院学报,2014,24(03):71-73.
[7]卢益,孙静,邓力.高效液相色谱质谱法测定地表水中丙烯酰胺[J].环境科学与技术,2012,35(12):136-138.
[8]吕康乐,宋俊密.溴化衍生-三重四极杆气质联用法测定地表水中丙烯酰胺[J].环境监测管理与技术,2016,28(02):55-56.
[9]尹燕敏,顾海东,秦宏兵.超高效液相色谱三重四极杆质谱联用法测定水中的丙烯酰胺[J].环境监控与预警,2012,12(04):20-22.
[10]付晓燕,李振国,包艳英,等.直接进样-超高效液相色谱-串联质谱测地表水中丙烯酰胺[J].中国环境监测,2014,30(05):77-79.
[11]中华人民共和国卫生部,中国国家标准化管理委员会.GB5749-2006.生活饮用水卫生标准[S].北京:中国标准出版社,2007.
[12]中华人民共和国环境保护部,环境保护部科技标准司.HJ697-2014.水质丙烯酰胺的测定气相色谱法[S].北京:中国标准出版社,2014.
[13]林现水.直接进样-超高效液相色谱-串联质谱测地表水中丙烯酰胺[J].环境监测,2014,91(07):61-62.
[14]中华人民共和国环境保护部,环境保护部科技标准司.HJ168-2010.分析方法标准制修订技术导则[S].北京:中国标准出版社,2010.