Simultaneous spectrophotometric determination of the residual of ciprofloxacin, famotidine, and tramadol using magnetic solid phase extraction coupled with multivariate calibration methods

Abstract In this work, a sensitive, simple, and inexpensive method have been developed based on magnetic solid Phase extraction for simultaneous spectrophotometric determination of ciprofloxacin (CIP), tramadol (TRA), and famotidine (FA) in the plasma, hospital waste, and river water. For this purpose, Fe3O4/GO-COOH nanocomposite was synthesized and characterized by Fourier transform infrared spectroscopy (FT-IR) and scanning electron microscopy (SEM). The effects of parameters on the extraction efficiency including pH, amount of sorbent, extraction time, elution solvent and its volume, and desorption time were evaluated and optimized. Under the optimal extraction conditions: 50mg of Fe3O4/GO-COOH nanocomposite, pH 5, extraction time 20 min, 20 mL of sample volume and eluting with 2 mL methanol: ammonium (0.2M) at 4 min, good linearity for CIP (0.03-1.5 mg L - 1 ), TRA (0.05-3 mg L - 1 ) and FA(0.05-3 mg L - 1 ) was obtained with an acceptable coefficient of determination (R2˃0.99). The absorption UV spectra of these drugs hardly overlap; thus, use of proper calibration methods is useful for their simultaneous spectrophotometric determination. After pre-concentration, partial least squares regression (PLS) as a multivariate calibration technique was utilized for analyzing the UV spectrum (240 - 320 nm) and simultaneous determination of drugs under the optimum condition. The results of the proposed method showed the low root mean square difference (RMSD) and high correlation coefficient (R2) of the prediction set of mixtures associated with the CIP, TRA, and FA. The developed method was also applied for simultaneous determination of three drugs in the spiked samples of plasma, hospital waste, and river water. The recoveries obtained by PLS lied within the range of 85%-101%.