Magnetic solid phase micro-extraction method with oxidized multiwalled carbon nanotube/Fe3O4 composite material for the analysis of trace 2,4,6-trinitrotoluen (TNT) in water samples by LC-MS/MS

DUMAN O., Aksoy Ç., TUNÇ S.

Microchemical Journal, cilt.218, 2025 (SCI-Expanded) identifier

  • Yayın Türü: Makale / Tam Makale
  • Cilt numarası: 218
  • Basım Tarihi: 2025
  • Doi Numarası: 10.1016/j.microc.2025.115577
  • Dergi Adı: Microchemical Journal
  • Derginin Tarandığı İndeksler: Science Citation Index Expanded (SCI-EXPANDED), Scopus, Academic Search Premier, BIOSIS, CAB Abstracts, Chemical Abstracts Core, Chimica, Food Science & Technology Abstracts, Index Islamicus, Veterinary Science Database
  • Anahtar Kelimeler: Liquid chromatography-tandem mass spectrometry, Magnetic oxidized MWCNT, Method development, Trinitrotoluene analysis, Validation, Water sample
  • Akdeniz Üniversitesi Adresli: Evet

Özet

The development of new reliable sensitive analytical methods for the detection of trace explosive substances in water samples is of great importance. In this study, magnetic oxidized multiwalled carbon nanotube (WMCNT)/Fe3O4 composite adsorbent material was fabricated by the oxidation of MWCNT with nitric acid and then by the coprecipitation of iron salts on the surface of oxidized MWCNT, and used for the first time in the magnetic solid phase micro-extraction of 2,4,6-trinitrotoluen (TNT) from various water samples prior to LC-MS/MS analysis. It was characterized using FTIR, BET specific surface area (169.0 m2 g−1), pore size distribution (mesopore volume: 0.852 cm3 g−1), SEM, EDS and VSM (saturation magnetization: 17.2 emu g−1) analyses. Analytical parameters affecting the extraction of TNT were optimized. The proposed method was of high sensitivity (LOD: 0.089 ng mL−1 and LOQ: 0.296 ng mL−1), acceptable accuracy, high selectivity and excellent precision in intra-day and inter-day (RSD (%) ≤ 2.96). TNT recovery values from ultra-pure water, tap water, synthetic wastewater and simulated cleaning cloth washing water were determined to be 85.8 %, 90.1 %, 65.9 % and 52.0 %, respectively. The presence of oil, organic matter and dust particles in the water samples led to a significant decrease in the recovery amounts of TNT. The results obtained from this study show that the proposed method is successful and reliable for the determination of trace levels of TNT in various water samples.