自制固相微萃取探针结合小型便携式质谱仪现场快速分析奶瓶洗液中6种酚类内分泌干扰物OA
On-site Rapid Analysis of Six Kinds of Phenolic Endocrine Disruptors in Baby Bottle Cleaning Solutions Using Custom-made Solid-phase Microextraction Probe Combined with A Miniature Mass Spectrometer
采用静电纺丝技术制备了聚丙烯腈/多壁碳纳米管(PAN/MWCNTs)固相微萃取(SPME)探针,并结合纳升萃取电喷雾离子化-小型便携式质谱技术建立了奶瓶洗液中6种酚类内分泌干扰物的现场快速检测方法.以不锈钢针作为 SPME探针的基底材料,采用静电纺丝技术在钢针表面依次修饰PAN和MWCNTs纳米材料,得到涂层为PAN/MWCNTs的萃取探针,微观结构表征结果表明,此探针涂层为网络状三维多孔结构.采用此探针对奶瓶洗液中的双酚A和4-叔丁基苯酚等6种酚类内分泌干扰物进行萃取富集,通过实验确定最佳的加热磁力搅拌器萃取温度为45℃、萃取时间为3 min、转速为400 r/min.萃取完成后,将探针插入含有10 μL乙腈的硼硅酸盐玻璃毛细管内,施加离子化电压,目标物即可被小型便携式质谱仪分析.6种内分泌干扰物的方法检出限为10~20 ng/mL,定量限为20~50 ng/mL,平均加标回收率为87.8%~106.9%,相对标准偏差为4.4%~11.2%,基质效应在0.95~1.02之间.本研究提出的基于不锈钢针制备PAN/MWCNTs探针的方法简单,探针稳定性强、萃取效率高;本方法简单、快速、准确、稳定,可在5 min内完成样品的快速检测,适用于奶瓶洗液中酚类内分泌干扰物的现场快速分析.
In this study,an on-site rapid detection method for 6 kinds of phenolic endocrine disruptors in baby bottle cleaning solution was established using solid-phase microextraction(SPME)coupled with nano-electrospray ionization and a miniature mass spectrometer.The polyacrylonitrile/multi-walled carbon nanotube(PAN/MWCNTs)coating of SPME probe was prepared by electrospinning.Using a stainless steel needle as the base material of the SPME probe,the coating of the PAN fibers and MWCNTs were successively modified on the surface of the steel needle and the microscopic structure indicated that the probe coating was a network-like three-dimensional porous structure.The probe was applied to extraction and enrichment of 6 kinds of phenolic endocrine disruptors,including bisphenol A and 4-tert-butylphenol,in baby bottle cleaning solution.The extraction temperature was set at 45℃with a stirring speed of 400 r/min and an extraction time of 3 min.After extraction,the probe was inserted into a borosilicate glass capillary containing 10 μL acetonitrile,and the ionization voltage was applied.The target substances were immediately analyzed by the miniature mass spectrometer.The limits of detection(LOD)and limits of quantification(LOQ)for the six kinds of endocrine disruptors were 10-20 ng/mL and 20-50 ng/mL,respectively.The recoveries were between 87.8%and 106.9%with the relative standard deviations(RSDs)from 4.4%to 11.2%,and the matrix effect was between 0.95 and 1.02.The streamlined analytical workflow was done within 5 min.The custom-made SPME probe had strong stability and high extraction efficiency.The developed method was simple,rapid,accurate and suitable for on-site rapid analysis of phenolic endocrine disruptors in baby bottle cleaning solutions.
郭项雨;郭德辉;朱惠欢;李纯;张婉茹;吕悦广;王斌;张庆
中国质量检验检测科学研究院,国家市场监督管理总局重点实验室(消费品质量安全与风险评估),北京 100176黄埔海关技术中心,广东省口岸安全智能化检测重点实验室,东莞 510510黄埔海关技术中心,广东省口岸安全智能化检测重点实验室,东莞 510510山东纳飞博科技发展有限公司,烟台 264000北京清谱科技有限公司,北京 100084中国质量检验检测科学研究院,国家市场监督管理总局重点实验室(消费品质量安全与风险评估),北京 100176黄埔海关技术中心,广东省口岸安全智能化检测重点实验室,东莞 510510中国质量检验检测科学研究院,国家市场监督管理总局重点实验室(消费品质量安全与风险评估),北京 100176
静电纺丝固相微萃取小型便携式质谱内分泌干扰物奶瓶洗液
ElectrospinningSolid-phase microextractionMiniature mass spectrometerEndocrine disruptorsBaby bottle cleaning solution
《分析化学》 2026 (7)
1237-1247,11
中央级公益性科研院所基本科研业务费专项资金项目(No.2024JK033)资助. Supported by the Basic Research Fund for Central Public Interest Institutes(No.2024JK033).
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