摘要
为了更加高效、快捷、经济地检测土壤中的邻苯二甲酸酯(PAEs),本文构建并优化了超声萃取-高效液相色谱(UE-HPLC)检测方法.选取美国环保署优先控制的邻苯二甲酸二甲酯、邻苯二甲酸二乙酯、邻苯二甲酸二正丁酯、邻苯二甲酸丁基苄基酯、邻苯二甲酸二(2-乙基己基)酯、邻苯二甲酸二正辛酯为实验对象,通过对6种PAEs的最大紫外吸收波长值进行测定、优化高效液相色谱运行条件,进而构建了土壤中6种PAEs的HPLC检测方法,具体参数如下:检测时间为30min;进样量为20µL;分离系统以乙腈-UP水为流动相、初始流速为1.0mL/min,采用梯度洗脱的方式分离PAEs,柱温为40;℃检测系统采用紫外检测器检测、开启波长切换模式,波长分别为205和290nm.采用线性回归方程及相关系数、加标回收率、相对标准偏差和检出限对方法进行评价.结果表明,该方法具有较宽的线性范围,最大质量浓度范围在0.1~100mg/L,相关系数均在0.999以上.1和5mg/kg的6种PAEs加标回收率范围分别为73.03%~91.89%和72.59%~90.70%,相对标准偏差范围分别为1.78%~12.46%和0.30%~7.56%.采用3倍噪音值法、液相色谱仪检定规程所得的6种PAEs检出限浓度范围分别为0.99~19.80和9.49~25.11µg/kg.
In order to detect phthalic acid esters(PAEs) in soils more efficiently, quickly and economically, an ultrasonic extraction-high-performance liquid chromatography(UE-HPLC) method was established and optimized. Dimethyl phthalate, diethyl phthalate, di-n-butyl phthalate, butyl benzyl phthalate, bis(2-ethylhexyl) phthalate, di-n-octyl phthalate were selected as experimental subjects, which were under the priority control of US Environmental Protection Agency. By measuring the maximum ultraviolet absorption wavelength of six types of PAEs and optimizing the operating conditions of high-performance liquid chromatography, the high-performance liquid chromatography detection method of six types of PAEs in soils was established. The specific parameters of the method are as follows: the detection time was 30min;the injection volume of the injection system was 20μL;the separation system used acetonitrile and ultrapure water as mobile phases, and the initial flow rate was 1.0mL/min. PAEs was separated by gradient elution, and the column temperature was 40℃. The detection system used ultraviolet detector to detect, and the wavelength switching mode was switched on, and the wavelength was 205 and 290nm respectively. The method was evaluated by linear regression equation, correlation coefficient, recovery rate, relative standard deviation and detection limit. The results showed that the method had a wide linear range, with the maximum mass concentration ranging from 0.1 to 100mg/L, and the correlation coefficients were above 0.999. The spiked recoveries of 1 and 5mg/kg were 73.03%~91.89% and 72.59%~90.70%, respectively, and the relative standard deviations were 1.78%~12.46% and 0.30%~7.56%. The detection limits of six types of PAEs were calculated by triple signal-to-noise ratio method and verification regulation of liquid chromatographs. The detection limits of PAEs were 0.99~19.80 and 9.49~25.11μg/kg, respectively.
作者
林家宝
孙雨豪
王建
高彦征
LIN Jia-bao;SUN Yu-hao;WANG Jian;GAO Yan-zheng(Institute of Organic Contaminant Control and Soil Remediation,College of Resources and Environment Science,Nanjing Agricultural University,Nanjing 210095,China;Jiangsu Environmental Engineering Technology Co.,Ltd.,Jiangsu Environmental Protection Group Co.,Ltd.,Nanjing 210019,China)
出处
《中国环境科学》
EI
CAS
CSCD
北大核心
2023年第2期756-763,共8页
China Environmental Science
基金
国家自然科学基金资助项目(42007104,22161132011)
江苏省碳达峰碳中和科技创新专项资金资助项目(20220013)。
关键词
高效液相色谱
邻苯二甲酸酯
土壤
检测方法
超声萃取
HPLC
phthalic acid esters(PAEs)
soil
detection method
ultrasonic extraction(UE)
