二硫化钼-氧化石墨烯纳米涂层针型微萃取装置联用气相色谱检测牛奶中5种多氯联苯  

Molybdenum disulfide-graphene oxide coated needle-type microextraction device combined gas chromatography for the determination of five kinds of polychlorinated biphenyls in milk

作　　者：赵金凤 张莹[1] 王希越[1] 娄大伟[1] ZHAO Jinfeng;ZHANG Ying;WANG Xiyue;LOU Dawei(College of Chemical and Pharmaceutical Engineering lin Institute of Chemical Technology,Jilin 132022,China)

机构地区：[1]吉林化工学院化学与制药工程学院,吉林132022

出　　处：《分析试验室》2025年第1期114-121,共8页Chinese Journal of Analysis Laboratory

基　　金：吉林省科技发展计划项目(202002008JC,20210509063RQ);吉林省产业技术研究与开发项目(2020C028-1);吉林省自然科学基金项目(YDZJ202201ZYTS460)资助。

摘　　要：利用溶剂热法合成二硫化钼-氧化石墨烯(MoS_(2)@GO)纳米材料作为涂层,通过溶胶凝胶法负载到直径为0.3 mm的不锈钢丝表面制得纤维,并将其填充到不锈钢针内,制成针型微萃取装置。与气相色谱(GC)联用,可用于牛奶中5种多氯联苯(PCBs)的萃取及分析。通过单因素实验确定最佳萃取条件:萃取温度90℃,萃取时间25 min,蠕动泵转速30 r/min,磁力搅拌器转速30 r/min,解吸温度270℃,解吸时间4 min,样品溶液盐浓度10%(w/V)。最优条件下,方法在0.025~200μg/L浓度范围内线性关系良好(r≥0.991),检出限范围为0.0072~0.0149μg/L,定量限范围在0.0239~0.0495μg/L之间,相对标准偏差(RSD)小于9.8%。将建立的方法应用于牛奶基质中PCBs的富集检测,加标回收率在80.2%~93.0%之间,RSD<8.2%。该方法为食品中PCBs的分析检测提供了一定的技术支撑。Molybdenum disulfide-graphene oxide(MoS_(2)@GO)nanomaterial was synthesized by the solvothermal method.The MoS_(2)@GO was loaded onto the surface of stainless-steel wire with a diameter of 0.3 mm by the solgel method.The prepared fiber was filled into a stainless-steel needle to make a needle-type microextraction device,which was combined with gas chromatography(GC)for the extraction of 5 kinds of polychlorinated biphenyls(PCBs)in milk.The optimal extraction conditions were determined by single factor experiment as follows:extraction temperature of 90℃,extraction time of 25 min,peristaltic pump speed of 30 r/min,magnetic stirrer speed of 30 r/min,desorption temperature of 270℃,desorption time of 4 min,and the amount of added salt of 10%(w/V).Under the optimal conditions,the linear relationship of the method was good(r≥0.991)in the concentration range of 0.025-200μg/L,the limits of detection were 0.0072-0.0149μg/L,the limits of quantification were0.0239-0.0495μg/L,and the relative standard deviations(RSDs)were less than 9.8%.The established method was applied to the enrichment of PCBs in milk.The recoveries ranged from 80.2%to 93.0%,and the RSDs were less than8.2%.This method can provide technical support for the analysis and detection of PCBs in food.

关 键 词：针型微萃取(NTME) MoS_(2)@GO纳米材料 气相色谱(GC) 多氯联苯(PCBs) 牛奶 

分 类 号：TS201.2[轻工技术与工程—食品科学]