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磁性复合材料的制备及其在水中多氯联苯测定中的应用OA

Preparation of Magnetic Composite Materials and Its Application in the Determination of PCBs in Water

中文摘要英文摘要

通过将聚多巴胺(PDA)包覆在磁性材料表面合成磁性复合材料NiFe2O4/SiO2@PDA,建立了一种磁固相萃取(MSPE)-气质联用快速测定水中18种多氯联苯(PCBs)的方法.称取0.05 g NiFe2O4/SiO2@PDA萃取剂,加入15.0 mL样品中(已调节样品pH 3.0),加入1.0 μL替代物标液,涡旋提取1.5 min,磁铁分离后倾出溶液,加入1.0 mL V(二氯甲烷)∶V(丙酮)=1∶1混合溶液,涡旋解吸2 min,磁铁分离后将溶液装入色谱小瓶中,至气质联用仪(GCMS)进行测定.方法学验证结果:18种PCBs的方法检出限为30~100 ng/L,相关系数r≥0.9995;对实际废水样品进行两个质量浓度(3.33、13.3 μg/L)的加标分析,加标回收率范围分别为91.8%~105%和92.8%~105%,相对标准偏差范围分别为1.7%~4.4%和1.6%~3.9%(n=6);磁性复合材料重复萃取6次后,目标物回收率93.1%~103%.该方法操作简单、快速、准确、可循环,可应用于水中18种PCBs的测定.

A magnetic composite material,NiFe2O4/SiO2@PDA,was synthesized by coating the surface of a magnetic material with polydopamine(PDA).A method for the rapid determination of 18 PCBs in water using magnetic solid-phase extraction coupled with gas chromatography-mass spectrometry(MSPE-GC-MS)was established.NiFe2O4/SiO2@PDA extractant(0.05 g)was added to water(15 mL;the pH of the sample was adjusted to 3.0),and a surrogate standard solution(1.0 μL)was added.The mixture was extracted by vortexing for 1.5 min,separated with a magnet,and the supernatant was decanted.Subsequently,1.0 mL of V(dichloromethane)∶V(acetone)=1∶1 was added,followed by vortex desorption for 2 min and a second separation with a magnet.The solution was transferred to a chromatographic vial and injected into a gas chromatography-mass spectrometer for determination.The method validation results were as follows:the method detection limits(MDLs)for the 18 PCBs ranged from 30 to 100 ng/L,with correlation coefficients(r)≥0.9995.Spiked recovery tests were performed on actual wastewater samples at two concentrations(3.33 and 13.3 μg/L).The spiked recoveries ranged from 91.8%to 105%and 92.8%to 105%,respectively,with relative standard deviations(RSDs)of 1.7%~4.4%and 1.6%~3.9%(n=6).After six repeated extractions using the magnetic composite material,the recoveries of the target analytes remained in the range of 93.1%~103%.This method is simple,rapid,accurate,recyclable,and can be applied to the determination of 18 PCBs in water.

王福德;张文舒

山东省沂水县检验检测中心,山东临沂 276400合肥综合性科学中心环境研究院,安徽 合肥 231299

化学化工

多氯联苯气质联用仪磁固相萃取废水聚多巴胺

PCBsGCMSMSPEwastewaterPDA

《化学试剂》 2026 (5)

54-61,8

10.13822/j.cnki.hxsj.2026.0014

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