Sandwich-structured MXene-Mn-MXene nanocomposite for vortex-assisted micro-solid phase extraction of lead in food and water samples
Microchemical Journal, cilt.230, 2026 (SCI-Expanded, Scopus)
- Yayın Türü: Makale / Tam Makale
- Cilt numarası: 230
- Basım Tarihi: 2026
- Doi Numarası: 10.1016/j.microc.2026.119943
- 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: Food analysis, Manganese intercalation, Sandwich-structured nanocomposite, Sorbent regeneration, Trace analysis
- Erciyes Üniversitesi Adresli: Evet
Özet
A vortex-assisted micro-solid-phase extraction (VA-μSPE) procedure based on a sandwich-structured MXene–Mn–MXene nanocomposite was developed for the determination of trace Pb(II) by high-resolution continuum-source flame atomic absorption spectrometry (HR-CS FAAS). XRD, FTIR, SEM–EDX, BET, and TGA characterization supported the formation of a Mn-containing layered MXene composite with improved accessible surface properties. Sorbent-free controls were used to distinguish sorbent-mediated extraction from pH-dependent Pb hydrolysis or precipitation. Under the optimized conditions—pH 7.0, 10 mg of sorbent, and 1 min of vortexing—the procedure processed a 40 mL sample and used 1.0 mL of 0.5 mol L−1 HCl for elution, providing a theoretical preconcentration factor of 40 and an experimental enrichment factor of 38.5. Recovery increased from 12.5% for the MAX-phase precursor and 74.8% for delaminated MXene to 99.1% for the fabricated composite, confirming the contribution of the composite architecture. The method achieved a limit of detection of 3.2 μg L−1, while intra- and interday relative standard deviations did not exceed 2.76%. Accuracy and practical applicability were verified using certified reference materials and water and food samples, with recoveries of 94.0–101.5%. The sorbent maintained at least 90.4% recovery through the first three extraction–desorption cycles, and no detectable Pb carryover was observed. Overall, the proposed VA-μSPE–HR-CS FAAS method provides a rapid, precise, and material-efficient approach for trace Pb(II) determination in complex samples.