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

作　　者：黄琼 刘媚嘉 朱群英[2] 马丽芳[2] 万佳丽 李良 HUANG Qiong;LIU Meijia;ZHU Qunying;MA Lifang;WAN Jiali;LI Liang(School of Ecology and Environment,Yuzhang Normal University,Nanchang 330103,China;Physical and Chemical Testing Department,Nanchang Center for Disease Control and Prevention,Nanchang 330038,China)

机构地区：[1]豫章师范学院生态与环境学院,南昌330103 [2]南昌市疾病预防控制中心理化检验科,南昌330038

出　　处：《理化检验(化学分册)》2025年第3期279-286,共8页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：江西省大学生创新创业训练计划项目(S202313774004,S202113774013);豫章师范学院高水平科研创新团队项目(YZTD202301)。

摘　　要：将苯胺甲基三乙氧基硅烷(AMTS)0.1 mL用N,N-二甲基甲酰胺(DMF)40 mL溶解,加入已制备好的Fe_(3)O_(4)NPs@SiO_(2)0.5 g,在110℃油浴中反应8 h。冷却至室温后,得到磁性纳米复合材料Fe_(3)O_(4)NPs@SiO_(2)-AMTS,依次用乙醇、水反复洗涤,于80℃真空干燥10 h。取经0.45μm水性滤膜过滤的水样10 mL,用盐酸调节pH至4.5左右,加入磁性纳米复合材料Fe_(3)O_(4)NPs@SiO_(2)-AMTS 20 mg,在室温下超声萃取20 min,并在外加磁场作用下弃去上清液。用乙腈1 mL将残渣超声解吸10 min,经0.45μm水性滤膜过滤后,采用高效液相色谱-质谱法测定滤液中邻苯二甲酸二正辛酯(DNOP)、邻苯二甲酸二甲酯(DMP)、邻苯二甲酸二(2-乙基己基)酯(DEHP)、邻苯二甲酸丁基苄基酯(BBP)、邻苯二甲酸二丁酯(DBP)和邻苯二甲酸二乙酯(DEP)6种邻苯二甲酸酯(PAEs)的含量。结果表明,6种PAEs的质量浓度均在1.000~2000μg·L^(−1)内与对应定量离子峰面积与内标定量离子峰面积的比值呈线性关系,检出限(3S/N)为0.0014~0.023μg·L^(−1)。按照标准加入法进行回收试验,回收率为66.0%~113%,优于HJ 1242—2022的回收率(70.0%~130%),测定值的日内相对标准偏差(RSD,n=6)和日间RSD(n=18)均小于15%。Aniline methyl triethoxysilane(AMTS,0.1 mL)was dissolved in 40 mL of N,N-dimethylformamide(DMF),and 0.5 g of prepared Fe_(3)O_(4)NPs@SiO_(2)was added,which reacted in an oil bath at 110℃for 8 h.After cooling to room temperature,magnetic nanocomposite material Fe_(3)O_(4)NPs@SiO_(2)-AMTS was obtained,which was washed repeatedly with ethanol and water,and dried in vacuum at 80℃for 10 h.10 mL of water sample filtered through a 0.45μm aqueous filter membrane was taken and adjusted to pH about 4.5 with hydrochloric acid,and 20 mg of magnetic nanocomposite material Fe_(3)O_(4)NPs@SiO_(2)-AMTS was 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 0.45μm 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 quantitative ion peak area and mass concentrations of 6 PAEs were found in the range of 1.000-2000μg·L^(−1),with detection limits(3S/N)in the range of 0.0014-0.023μg·L^(−1).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%.

关 键 词：磁性纳米复合材料 高效液相色谱-质谱法 邻苯二甲酸酯 环境水体 

分 类 号：O657.63[理学—分析化学]