A green ultrasonic-assisted micro solid-phase extraction of Zn and Cd on manganese molybdate-modified copper(II) aluminate nanocomposite from wastewater and cosmetic products


AHMED H. E. H., Çoban A. N., SOYLAK M.

Microchemical Journal, cilt.228, 2026 (SCI-Expanded, Scopus)

  • Yayın Türü: Makale / Tam Makale
  • Cilt numarası: 228
  • Basım Tarihi: 2026
  • Doi Numarası: 10.1016/j.microc.2026.119084
  • Dergi Adı: Microchemical Journal
  • Derginin Tarandığı İndeksler: Science Citation Index Expanded (SCI-EXPANDED), Scopus, BIOSIS, Chemical Abstracts Core, Chimica, Index Islamicus, Academic Search Ultimate (EBSCO), Engineering Source (EBSCO)
  • Anahtar Kelimeler: Cosmetics, CuAl₂O₄@MnMoO₄ nanocomposite, Flame atomic absorption spectrometry, Ultrasonic-assisted micro-solid phase extraction (UA-μSPE), Wastewater, Zn(II) and Cd(II)
  • Erciyes Üniversitesi Adresli: Evet

Özet

Accurate, sensitive, and eco-friendly sample preparation methods are needed for trace levels of hazardous and essential metal ions in environmental water and cosmetic products before instrumental analysis. The development of effective miniature extraction methods is important for minimizing matrix interference, enhancing analytical sensitivity, and decreasing solvent utilization. In this work, a novel ultrasonic-assisted micro-solid-phase extraction (UA-μSPE) method coupled with flame atomic absorption spectrometry (FAAS) was developed for the simultaneous preconcentration, separation, and determination of Zn(II) and Cd(II) in wastewater and cosmetic products using a new nanocomposite (CuAl₂O₄@MnMoO₄) as the adsorbent. The nanocomposite was prepared using a combined sol-gel and hydrothermal method and characterized by X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FTIR), field emission scanning electron microscopy with energy-dispersive X-ray spectroscopy (FE-SEM/EDX), and thermogravimetric analysis-differential thermal analysis (TGA-DTA). Important variables influencing extraction efficiency, such as pH, quantities of adsorbent and ligand, contact and elution durations, sample volume, and type/concentration of eluent, were optimized. Under optimal conditions (pH 7.5, 5 mg adsorbent, 30 μg PAN ligand, 1 min sonication, 1 mL of 0.1 mol L⁻¹ HNO₃ elution), the method achieved low detection limits (1.24 μg kg⁻¹ for Zn, 0.48 μg kg⁻¹ for Cd), high preconcentration factor of 40, and excellent reusability (up to 10 cycles). The pHpzc of the nanocomposite was measured at 6.2. Validation using certified reference materials (BCR Estuarine Water 505 and NIST 1573a Tomato Leaves) showed high concordance with certified values. The suggested UA-μSPE-FAAS method was successfully applied to real tap water, wastewater, and cosmetic samples (lotions, toothpaste, and sunscreen) with quantitative recoveries (85–105%). Sustainability evaluations were done using AGREEprep (score 0.61) and White Analytical Chemistry (total score 81), which point out the method's high compatibility with green analytical chemistry concepts.