Page 52 - 理化检验-化学分册2025年第三期

黄 琼，等：基于磁性纳米复合材料的高效液相色谱-质谱法测定环境水体中6种邻苯二甲酸酯的含量

Determination of 6 Phthalate Esters in Environmental Water Body by High
Performance Liquid Chromatography-Mass Spectrometry
Based on Magnetic Nanocomposite Materials

HUANG Qiong , LIU Meijia , ZHU Qunying , MA Lifang , WAN Jiali , LI Liang 1*
2
1
2
1
1
(1. School of Ecology and Environment, Yuzhang Normal University, Nanchang 330103, China;
2. Physical and Chemical Testing Department, Nanchang Center for Disease Control and Prevention, Nanchang 330038, China)
Abstract: Aniline methyl triethoxysilane (AMTS, 0.1 mL) was dissolved in 40 mL of N, N-dimethylformamide (DMF),
and 0.5 g of prepared Fe O NPs@SiO was added, which reacted in an oil bath at 110 ℃ for 8 h. After cooling to room temperature,
3 4 2
magnetic nanocomposite material Fe O NPs@SiO -AMTS was obtained, which was washed repeatedly with ethanol and water,
3 4 2
and dried in vacuum at 80 ℃ for 10 h. 10 mL of water sample filtered through a 0.45 µm aqueous filter membrane was taken and
adjusted to pH about 4.5 with hydrochloric acid, and 20 mg of magnetic nanocomposite material Fe O NPs@SiO -AMTS was
3 4 2
added, which was extracted by ultrasound at room temperature for 20 min. The supernatant was discarded under the action of
an external magnetic field. The residue was desorbed by ultrasound with 1 mL of acetonitrile for 10 min, the solution obtained
was filtered through a 0.45 µm aqueous filter membrane, and high performance liquid chromatography-mass spectrometry was
used to determine 6 phthalates ester (PAEs) in the filtrate, including di-n-octyl phthalate (DNOP), dimethyl phthalate (DMP),
di(2-ethylhexyl) phthalate (DEHP), butyl benzyl phthalate (BBP), dibutyl phthalate (DBP), and diethyl phthalate (DEP). As
shown by the results, linear relationships between the ratios of the corresponding quantitative ion peak area to the internal standard
−1
quantitative ion peak area and mass concentrations of 6 PAEs were found in the range of 1.000-2 000 μg · L , with detection limits
−1
(3S/N) in the range of 0.001 4-0.023 μg · L . Test for recovery was made by the standard addition method, giving the results in
the range of 66.0%-113%, which was better than those of HJ 1242—2022 (70.0%-130%). RSDs of the determined values for
inter-day (n=6) and intra-day (n=18) were less than 15%.
Keywords: magnetic nanocomposite material; high performame liquid chromatography-mass spectrometry; phthalate ester;
environmental water body

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