Stir bar sorptive extraction and liquid chromatography with UV detection for determination of antidepressants in plasma samples

Departamento de Química, Faculdade de Filosofia, Ciências e Letras de Ribeirão Preto, Universidade de São Paulo, Ribeirão Preto, SP 14040-901, Brazil.
Journal of Chromatography B (Impact Factor: 2.73). 06/2007; 850(1-2):295-302. DOI: 10.1016/j.jchromb.2006.11.042
Source: PubMed


A sensitive and reproducible stir bar sorptive extraction and liquid chromatography (SBSE/LC-UV) method is described for the determination of sertraline, mirtazapine, fluoxetine, citalopram, paroxetine, imipramine, nortriptyline, amitriptyne, and desipramine in plasma samples. Important factors in the optimization of SBSE efficiency are discussed, such as extraction time, pH, ionic strength, influence of plasma proteins, and desorption conditions: solvents, modes (magnetic stir, ultrasonic), time, and number of desorption steps. The SBSE/LC-UV method showed to be linear in a concentration ranging from the limit of quantification (LOQ) to 1000.0 ng mL(-1). The LOQ values ranged from 10.0 ng mL(-1) to 40.0 ng mL(-1). The inter-day precision of the SBSE/LC-UV method presented coefficient of the variation lower than 15%. Based on figures of the merit results, the SBSE/LC-UV methodology showed to be adequate to the antidepressants analyses from therapeutic to toxic therapeutic levels. In order to evaluate the proposed method for clinical use, the SBSE/LC-UV method was applied to the analysis of plasma samples from elderly depressed patients.

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    • "To overcome this limitation, SBSE emerged [4] [11]. The main limitation of SBSE is that, till very recently, only one non-polar coating based on poly(dimethylsiloxane) (PDMS) was commercially available, which showed excellent performance for the sorption of non-polar analytes but most of the polar analytes were not retained at all or retained poorly [15] [16] [17]. Nevertheless, in the last years, two new SBSE polar coatings have been commercially available and trademarked as Acrylate Twister ® (based on polyacrylate with proportion of polyethylene glycol) and EG/Silicone Twister ® (based on polyethylene glycol modified with silicone). "
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    ABSTRACT: A new sorptive extraction technique, fabric phase sorptive extraction (FPSE), using different coating chemistries: non-polar sol-gel poly(dimethyldiphenylsiloxane) (PDMDPS), medium polar sol-gel poly(tetrahydrofuran) (PTHF), and polar sol-gel poly(ethylene glycol)-block-poly(propylene glycol)-block-poly(ethylene glycol) (PEG-PPG-PEG triblock) and sol-gel Carbowax 20M were evaluated to extract a group of pharmaceuticals and personal care products (PPCPs) with wide range of polarity from environmental aqueous samples. Different parameters affecting FPSE such as sample pH, stirring speed, addition of salt, extraction time, sample volume, elution solvent and desorption time were optimized for each sorbent coated FPSE media. Under optimum conditions, FPSE media coated with sol-gel Carbowax 20M provided the highest absolute recoveries (77-85%) for majority of the analytes with the exception of the most polar ones. Nevertheless, all four sorbents offered better recovery compared to the commercially available coating for stir-bar sorptive extraction based on Ethylene Glycol/Silicone (EG/Silicone). The method based on FPSE with sol-gel Carbowax 20M media and liquid chromatography–(electrospray ionization) tandem mass spectrometry (LC-(ESI) MS/MS) was developed and validated for environmental water samples. Good apparent recoveries (41 - 80%), detection limits (1 - 50 ng L -1 ), repeatability (%RSD<15%, n=5) and reproducibility (%RSD<18%, n=5) were achieved.
    Talanta 08/2015; 144. DOI:10.1016/j.talanta.2015.08.009 · 3.55 Impact Factor
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    • "This process reduces the extraction time and increase the EFs (Rahnama Kozani et al., 2007). SPME (Ulrich and Martens, 1997), SBSE (Chaves et al., 2007) and DLLME (Yazdi et al., 2008) have been used as sample preparation techniques in the determination of some antidepressants. Combination of derivatiation and DLLME can reduce analysis time and/or increase the extractability of the analytes. "
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    ABSTRACT: This paper presents a fast and simple method for the extraction, preconcentration and determination of fluvoxamine, nortriptyline and maprotiline in urine using simultaneous derivatization and temperature-assisted dispersive liquid–liquid microextraction (TA-DLLME) followed by gas chromatography–flame ionization detection (GC-FID). An appropriate mixture of dimethylformamide (disperser solvent), 1,1,2,2-tetrachloroethane (extraction solvent) and acetic anhydride (derivatization agent) was rapidly injected into the heated sample. Then the solution was cooled to room temperature and cloudy solution formed was centrifuged. Finally a portion of the sedimented phase was injected into the GC-FID. The effect of several factors affecting the performance of the method, including the selection of suitable extraction and disperser solvents and their volumes, volume of derivatization agent, temperature, salt addition, pH and centrifugation time and speed were investigated and optimized. Figures of merit of the proposed method, such as linearity (r2 > 0.993), enrichment factors (820–1070), limits of detection (2–4 ng mL−1) and quantification (8–12 ng mL−1), and relative standard deviations (3–6%) for both intraday and interday precisions (concentration = 50 ng mL−1) were satisfactory for determination of the selected antidepressants. Finally the method was successfully applied to determine the target pharmaceuticals in urine. Copyright © 2014 John Wiley & Sons, Ltd.
    Biomedical Chromatography 12/2014; 29(7). DOI:10.1002/bmc.3396 · 1.72 Impact Factor
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    • " consuming and require large amounts of organic solvents [4]. "
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    ABSTRACT: This paper describes a new approach for the determination of amitriptyline in wastewater by ionic liquid based immersed droplet microextraction (IL-IDME) prior to high-performance liquid chromatography with ultraviolet detection. 1-Hexyl-3-methylimidazolium hexafluorophosphate ([C6MIM][PF6]) was used as an ionic liquid. Various factors that affect extraction, such as volume of ionic liquid, stirring rate, extraction time, pH of the aqueous solution and salting effect, were optimized. The optimal conditions were as follows: microextraction time, 10 min; stirring rate, 720 rpm; pH, 11; ionic drop volume, 100 μL; and no sodium chloride addition. In quantitative experiments the method showed linearity in a range from 0.01 to 10 μg/mL, a limit of detection of 0.004 μg/mL and an excellent pre-concentration factor (PF) of 1100. Finally, the method was successfully applied to the determination of amitriptyline in the hospital wastewater samples.
    Journal of Pharmaceutical Analysis 10/2012; 2(5):361–365. DOI:10.1016/j.jpha.2012.07.007
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