Rapid determination of tramadol in human plasma by headspace solid-phase microextraction and capillary gas chromatography-mass spectrometry.
ABSTRACT A simple, rapid and sensitive method for determination of tramadol in plasma samples was developed using headspace solid-phase microextraction (HS-SPME) and gas chromatography with mass spectrometry (GC-MS). The optimum conditions for the SPME procedure were: headspace extraction on a 65-microm polydimethylsiloxane/divinylbenzene (PDMS/DVB) fiber; 0.5 mL of plasma modified with 0.5 mL of sodium hydroxide (0.1 M); extraction temperature of 100 degrees C, with stirring at 2000 rpm for 30 min. The calibration curve showed linearity in the range of 1-400 ng mL(-1) with regression coefficient corresponding to 0.9986 and coefficient of the variation of the points of the calibration curve lower than 10%. The detection limit for tramadol in plasma was 0.2 ng mL(-1). The proposed method was successfully applied to determination of tramadol in human plasma samples from 10 healthy volunteers after a single oral administration.
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ABSTRACT: Tramadol is an opioid, synthetic analog of codeine and has been used for the treatment of acute or chronic pain may be abused. In this work, a developed Dispersive liquid liquid microextraction (DLLME) as binary solvents-based dispersive liquid-liquid microextraction (BS-DLLME) combined with high performance liquid chromatography (HPLC) with fluorescence detection (FD) was employed for determination of tramadol in the urine samples. This procedure involves the use of an appropriate mixture of binary extraction solvents(70 muL CHCl3 and 30 muL ethyl acetate) and disperser solvent (600 muL acetone) for theformation of cloudy solution in 5 ml urine sample comprising tramadol and NaCl (7.5%, w/v). After centrifuging, the small droplets of extraction solvents were precipitated. In the final step, the HPLC with fluorescence detection was used for determination of tramadol in the precipitated phase. Various factors on the efficiency of the proposed procedure were investigated and optimized. The detection limit (S/N = 3) and quantification limit (S/N = 10) were found 0.2 and 0.9 mug/L, respectively. The relative standard deviations (RSD) for the extraction of 30 mug L of tramadol was found4.1% (n = 6). The relative recoveries of tramadol from urine samples at spiking levels of 10, 30and60 mug/L were in the range of 95.6 - 99.6%. The relative recoveries of tramadol from urine samples at spiking levels of 10, 30, 60 mug/ L were in the range of95.6 - 99.6%. Compared with other methods, this method provides good figures of merit such as good repeatability, high extraction efficiency, short analysis time, simple procedure and can be used as microextraction technique for routine analysis in clinical laboratories.DARU-JOURNAL OF FACULTY OF PHARMACY 02/2014; 22(1):25. · 0.62 Impact Factor
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ABSTRACT: Electrospun nanofibers from poly(methylmethacrylate) (PMMA) and polystyrene (PS) blend were used as a sorbent to extract tramadol from urine and plasma samples. Then, the tramadol concentration was determined by corona discharge ion mobility spectrometry. The hydrophilic (PMMA) and hydrophobic (PS) properties of the blend polymer improved extraction efficiency of the analyte. The scanning electron microscopy images of the PMMA/PS nanofibers showed a diameter range of 130–600 nm with a smooth morphology. Parameters affecting extraction efficiency were optimized and under the optimized conditions, the dynamic ranges and detection limit of tramadol were found to be 30–500 and 10–200 ng mL−1, and 9.4 and 1.6 ng mL−1 in plasma and urine samples, respectively.Chromatographia 76(9-10). · 1.44 Impact Factor
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ABSTRACT: In this work a novel procedure based on surfactant-assisted directly suspended droplet microextraction for the determination of tramadol prior to GC with flame ionization detection is proposed. In this technique, a free microdroplet of solvent is transferred to the surface of an immiscible aqueous sample containing Triton X-100 and tramadol while being agitated by a stirring bar placed on the bottom of the sample vial. After the predetermined time, the microdroplet of solvent is withdrawn by a syringe and analyzed. The effective parameters such as the type of organic solvent, extraction time, microdroplet volume, salt content of the donor phase, stirring speed, the source phase pH, concentration of Triton X-100 and extraction temperature were optimized. For this purpose, a multivariate strategy was applied based on an experimental design in order to screen and optimize the significant factors. This method requires minimal sample preparation, analysis time, and solvent consumption and represents significant advantages over customary analytical methods. The linearity ranged from 10-2000 μg L(-1) with relative standard deviations (n = 5) of 7.3-10. Preconcentration factors and the limits of detection were 391-466 and 2.5-6.5 μg L(-1) , respectively. Finally, this method was applied to the analysis of biological samples, and satisfactory results were obtained. This article is protected by copyright. All rights reserved.Journal of Separation Science 09/2013; · 2.59 Impact Factor