Study on the high-performance liquid chromatography detection method of phthalic acid esters in soils
LIN Jia-bao1,2, SUN Yu-hao1, WANG Jian1, GAO Yan-zheng1
1. Institute of Organic Contaminant Control and Soil Remediation, College of Resources and Environment Science, Nanjing Agricultural University, Nanjing 210095, China; 2. Jiangsu Environmental Engineering Technology Co., Ltd., Jiangsu Environmental Protection Group Co., Ltd., Nanjing 210019, China
Abstract：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 20 μL; 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.
林家宝, 孙雨豪, 王建, 高彦征. 土壤中邻苯二甲酸酯的高效液相色谱检测方法[J]. 中国环境科学, 2023, 43(2): 756-763.
LIN Jia-bao, SUN Yu-hao, WANG Jian, GAO Yan-zheng. Study on the high-performance liquid chromatography detection method of phthalic acid esters in soils. CHINA ENVIRONMENTAL SCIENCECE, 2023, 43(2): 756-763.
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