摘要
建立了水质中邻苯二甲酸二甲酯(DMP)、邻苯二甲酸二丁酯(DBP)、邻苯二甲酸二辛酯(DOP)的前处理及反相超高效液相色谱检测方法,通过单因素试验考察了色谱柱类型、流动相类型、流动相体积分数、流速及柱温对主峰信噪比的影响,并采用响应面分析法进行了方案优化。结果表明:氰基色谱柱优于C 18色谱柱;在最优色谱条件(流动相乙腈水溶液(体积分数64%)、流速0.22 mL/min、柱温28℃)下,DMP、DBP、DOP的主峰信噪比平均值分别为8890、6637、2991,对应的检出限分别为0.05、0.03、0.08μg/L,均低于《水质邻苯二甲酸二甲(二丁、二辛)酯的测定液相色谱法》(HJ/T 72—2001)规定的检出限,加标回收率分别为98.4%、99.8%和98.0%,相对标准偏差为0.98%、0.52%和0.83%,具有良好的灵敏度、回收率和重复性,能更好满足地下水等水体的痕量检测要求。
A method for pretreatment and determination of ultrahigh performance liquid chromatography of dimethyl phthalate(DMP),dibutyl phthalate(DBP)and dioctyl phthalate(DOP)in water was established.The effects of column type,mobile phase type,mobile phase volume fraction,flow rate and column temperature on the signal noise ratio of main peak were investigated by single factor test,and the scheme was optimized by response surface methodology.The results showed that cyanide column was better than C 18 column.Under the optimal chromatographic conditions(mobile phase acetonitrile aqueous solution(volume fraction 64%),flow rate 0.22 mL/min,column temperature 28℃),the signal noise ratios of main peak of DMP,DBP and DOP were 8890,6637 and 2991 respectively.The corresponding detection limits were 0.05,0.03 and 0.08μg/L respectively,all lower than the detection limit specified in“Water quality-determination of phthalate(dimethyl dibutyl dioctyl)-liquid chromatography”(HJ/T 72-2001).The recovery rate of spiking were 98.4%,99.8%and 98.0%,respectively,and the relative standard deviation was 0.98%,0.52%and 0.83%,which had good sensitivity,recovery and repeatability,and could better meet the requirements for trace detection of groundwater and other water bodies.
作者
孔彬
黄志鹏
杜健鹏
刘至能
吴启航
陈莉娜
KONG Bin;HUANG Zhipeng;DU Jianpeng;LIU Zhineng;WU Qihang;CHEN Lina(Guangzhou Inspection,Testing and Certification Group Co.,Ltd.,Guangzhou Guangdong 511447;School of Civil Engineering,Guangzhou University,Guangzhou Guangdong 510006;College of Environmental Science and Engineering,Guangzhou University,Guangzhou Guangdong 510006;Key Laboratory of Water Quality Safety and Protection of Pearl River Delta,Ministry of Education,Guangzhou Guangdong 510006;Guangdong Engineering and Technology Center of Comprehensive Control of Rural Water Environment Non-point Source Pollution,Guangzhou Guangdong 510006;Collaborative Innovation Laboratory of Soil Environment,Guangzhou Guangdong 510006;School of Geography Science,Hunan Normal University,Changsha Hunan 410081)
出处
《环境污染与防治》
CAS
CSCD
北大核心
2023年第3期376-383,407,共9页
Environmental Pollution & Control
基金
国家重点研发计划项目(No.2020A0607142)
教育部产学合作协同育人项目(No.202101134012、No.202102201012)
广州检验检测认证集团有限公司科研项目“超高效液相色谱法测定水质中邻苯二甲酸酯类的方法研究”(No.2019kj02GK)。
关键词
响应面分析法
邻苯二甲酸酯
超高效液相色谱
response surface methodology
phthalate acid esters
ultrahigh performance liquid chromatography
作者简介
第一作者:孔彬,男,1987年生,本科,高级工程师,研究方向为水土环境中的有机污染;通讯作者:吴启航。
