Layered double hydroxide intercalated with tyrosine for ultrasonic-assisted microextraction of tramadol and methadone from biological samples followed by GC/MS analysis.

A magnetic nanocomposite adsorbent based on Zn-Al layered double hydroxide (LDH) intercalated with tyrosine has been synthesized for ultrasound-assisted extraction of two drugs of abuse: tramadol (TRA) and methadone (MET). Analysis was carried out using gas chromatography-mass spectrometry. The synthesized LDH was characterized by Fourier transform-infrared spectroscopy, X-ray diffraction, field emission scanning electron microscopy, and energy-dispersive X-ray spectroscopy. The most important extraction parameters such as type of the elution solvent, pH value of the sample solution, and the amount of the adsorbent were optimized. With assistance of ultrasound radiation, the maximum extraction of target drugs using the fabricated LDH was achieved within 5 min. Under the optimized conditions, the limits of determination were 0.45, 0.45, 2.5, and 0.8 µg L-1 for TRA and 0.15, 0.15, 1.2, and 0.5 µg L-1 for MET in water, urine, plasma, and saliva samples, respectively. The preconcentration factors obtained were in the range of 50-145. The matrix effect for MET and TRA is considerable in plasma (66%, 18%) and saliva (72%, 34%), respectively. The precision was found to be better 11% RSD. The maximum adsorption capacity is 4.84 (mg g-1) (L mg-1)1/n based on the Freundlich isotherm. The proposed method presents good results for trace determination of tramadol and methadone in biological samples with satisfactory repeatability. Graphical abstract.