Rapid extraction of BTEX in water and milk samples based on functionalized multi-walled carbon nanotubes by dispersive homogenized-micro-solid phase extraction.

An advanced synthesis based on the phenylalanine (Phe) and task-specific ionic liquid (TSIL) functionalized on multi-walled carbon nanotubes (Phe/TSIL@MWCNTs), was used to extract benzene, ethylbenzene, toluene, and xylene (BTEX) from cow's milk, powdered milk, and farm water samples. The BTEX was efficiently extracted by ultrasound-assisted dispersive homogenized-micro-solid phase extraction (USA-DH-µ-SPE) between 95.1% and 103.4%. By procedure, 50 mg of Phe/TSIL@MWCNTs was added to 0.2 mL of acetone and injected into 10 mL of the samples. The upper aqueous solution was vacuumed, the vial heated to 80 °C, and the BTEX desorbed in the vial. Then, using a Hamilton syringe, 1-20 µL of gas in the headspace vial was determined by injecting it into the gas chromatography with flame ionization detection (GC-FID). The linear range, LOD, and LOQ for BTEX in milk and water samples were obtained at 0.05-500 µg L-1, 15 ng L-1, and 50 ng L-1, respectively (r = 0.9997, RSD% = 2.27).

An immobilization of aminopropyl trimethoxysilane-phenanthrene carbaldehyde on graphene oxide for toluene extraction and separation in water samples.

A new functionalized Nano graphene with aminopropyl trimethoxysilane-phenanthrene-4-carbaldehyde (NGO@APTMS-PNTCA) as a novel adsorbent was used to extract toluene from water samples by the ultrasound-assisted dispersive solid-phase microextraction procedure (USA-D-SPME). So, 50 mg of NGO@APTMS-PNTCA adsorbent was added to water samples and sonicated for 20 min. After toluene extraction, the NGO@APTMS-PNTCA adsorbent separated from the liquid phase with a Whatman membrane filter (200 nm). Then, the toluene was back-extracted from the adsorbent by 2.0 mL of the acetone/ethanol (1:1, eluent) at 25 °C. Due to the physical properties and structure of toluene, fluorobenzene was used as an internal standard. Finally, the toluene values were measured by a gas chromatography-flame ionization detector (GC-FID). In optimized conditions, the limit of detection (LOD), the working range (WR), and the enrichment factor (EF) were obtained at 2.5 µg L-1, 0.01-1.2 mg L-1, and 9.63, respectively (MRSD% = 3.38). Also, the limit of quantification (LOQ) 10 µg L-1 and extraction recovery of more than 95% was efficiently achieved for toluene. Standard additions of toluene to blank solutions had high recoveries between 95.2% and 104.5% with a relative standard deviation (RSD%) of 0.27-5.2. The absorption capacities of NGO and NGO@APTMS-PNTCA adsorbents for toluene extraction were obtained at 32.8 mg g-1 and 154.9 mg g-1, respectively. The USA-D-SPME method was validated by spiking the standard concentrations of toluene. The proposed method demonstrated relevant and suitable statistical results with high accuracy and precision for toluene extraction by a novel adsorbent synthesis.