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氧化石墨烯掺杂聚丙烯腈-马来酸共聚物纳米纤维用于高效液相色谱法测定牛奶中的阿莫西林和土霉素

Graphene oxide doped polyacrylonitrile-co-maleic acid nanofibers for high-performance liquid chromatography determination of amoxicillin and Oxytetracycline in milk.

作者信息

Mohamed Shaymaa A, Alahmad Waleed, Darwish Ibrahim A, Aly Saad Aly Mohamed, Varanusupakul Puttaruksa

机构信息

Department of Chemistry, Faculty of Science, Chulalongkorn University, Bangkok, 10330, Thailand.

Department of Pharmaceutical Chemistry, College of Pharmacy, King Saud University, P.O. Box 2457, Riyadh, 11451, Saudi Arabia.

出版信息

Sci Rep. 2025 May 24;15(1):18128. doi: 10.1038/s41598-025-00356-0.

Abstract

Detecting and quantifying trace amounts of antibiotics like amoxicillin and oxytetracycline in milk and environmental water samples is crucial for public health and environmental monitoring. This research focuses on developing a novel sorbent for solid-phase extraction (SPE) of amoxicillin and oxytetracycline from milk and environmental water samples, using electrospun graphene oxide-doped poly(acrylonitrile-co-maleic acid) nanocomposite fibers, followed by high-performance liquid chromatography with diode array detection (HPLC-DAD). The fibers were successfully fabricated and characterized using a suite of techniques: SEM-EDX, FTIR, XRD, BET, XPS, TGA, and Raman spectroscopy. The extraction process was optimized by carefully adjusting parameters like desorption solvent (0.60 mL of 0.2 M HCl in methanol), extraction time (60 min), and sample pH (3) to achieve efficient and reliable extraction. Under optimal conditions, the developed method demonstrated good linearity (5-100 µg/L, R² > 0.9925), low detection and quantification limits (1.50 µg/L and 5.0 µg/L for amoxicillin and 1.46 µg/L and 4.8 µg/L for oxytetracycline) and high enrichment factor (21 for amoxicillin and 47 for oxytetracycline). The achievable accuracy and precision of the developed sorbent were satisfying, for incidence, relative recovery range of 90.3-106.3% and 87.6-95.9% with RSD range of 1.9-4.3% and 1.1-4.7% for amoxicillin and oxytetracycline, respectively. The method demonstrates reliable and efficient extraction and quantification of antibiotics from two different classes at maximum residue levels, making it suitable for monitoring antibiotic contamination in food and environmental samples, ultimately promoting better public health outcomes.

摘要

检测和定量牛奶及环境水样中的痕量抗生素,如阿莫西林和土霉素,对于公共卫生和环境监测至关重要。本研究聚焦于开发一种新型吸附剂,用于从牛奶和环境水样中固相萃取(SPE)阿莫西林和土霉素,采用电纺氧化石墨烯掺杂聚(丙烯腈 - 马来酸)纳米复合纤维,随后结合二极管阵列检测高效液相色谱法(HPLC - DAD)。通过扫描电子显微镜 - 能谱仪(SEM - EDX)、傅里叶变换红外光谱仪(FTIR)、X射线衍射仪(XRD)、比表面积分析仪(BET)、X射线光电子能谱仪(XPS)、热重分析仪(TGA)和拉曼光谱仪等一系列技术成功制备并表征了这些纤维。通过仔细调整解吸溶剂(0.60 mL含0.2 M HCl的甲醇溶液)、萃取时间(60分钟)和样品pH值(3)等参数对萃取过程进行了优化,以实现高效可靠的萃取。在最佳条件下,所开发的方法显示出良好的线性(5 - 100 μg/L,R² > 0.9925)、低检测限和定量限(阿莫西林的检测限为1.50 μg/L,定量限为5.0 μg/L;土霉素的检测限为1.46 μg/L,定量限为4.8 μg/L)以及高富集因子(阿莫西林为21,土霉素为47)。所开发吸附剂的准确度和精密度令人满意,例如,阿莫西林的相对回收率范围为90.3 - 106.3%,相对标准偏差(RSD)范围为1.9 - 4.3%;土霉素的相对回收率范围为87.6 - 95.9%,RSD范围为1.1 - 4.7%。该方法证明了在最大残留水平下从两类不同抗生素中进行可靠且高效的萃取和定量,使其适用于监测食品和环境样品中的抗生素污染,最终促进更好的公共卫生结果。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/76fe/12103578/cd4fd1d5afc0/41598_2025_356_Fig1_HTML.jpg

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