Rapid determination of tramadol in human plasma by headspace solid-phase microextraction and capillary gas chromatography-mass spectrometry
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.
Available from: Hoda Lavasani
- "However, LLE is time consuming and requires large amounts of organic solvent and SPE uses much less than LLE, but can be relatively expensive. Recently, other extraction methods as free solvent and miniaturized extractions, such as liquid phase microextraction (LPME)
[10,11], solid phase microextraction (SPME)
, solvent bar microextraction (SBME)
, liquid phase microextraction with back extraction (LPME-BS)
, three - phase hollow fiber liquid phase microextraction (HF-LPME)
, have successfully been developed for determination of tramadol from different matrices. Dispersive liquid-liquid microextraction (DLLME) is a miniaturized liquid extraction that was introduced in 2006 by Rezaee and coworkers
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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.
Available from: Ali Esrafili
- "Several analytical methods such as gas chromatography (GC) coupled to nitrogen selective or even mass-spectrometry detection , capillary electrophoresis  and high performance liquid chromatography (HPLC) with electrochemical , mass spectrometry  or fluorescence detectors  have been introduced for separation and determination of tramadol. Usually, an initial sample preparation step is essential for isolation and preconcentration of tramadol in biological samples prior to its final analysis. "
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ABSTRACT: The aim of this research was to compare the extraction efficiencies of two modes of three-phase hollow fiber microextraction (HF-LLLME) based on aqueous and organic acceptor phases for analysis of tricyclic antidepressant (TCA) drugs. High-performance liquid chromatography with photodiode array detection (HPLC-DAD) was applied for determination of the drugs. In order to examine the ability of the new concept of HF-LLLME based on organic acceptor solvent in comparison with aqueous acceptor phase to extract the analytes, four TCAs were selected. The effect of different extraction conditions (i.e., type of acceptor phase, hollow fiber length, ionic strength, stirring rate, and extraction time) on the extraction efficiency of the TCAs was investigated and optimized using central composite design (CCD) as a powerful tool. Both methods were characterized by good linearity and high repeatability, but HF-LLLME with organic acceptor provided higher extraction efficiency and thus lower limits of detection (LODs). Calibration curves were linear (r(2)>0.996) in the range of 0.2-200 μgL(-1). LODs for all the TCAs ranged from 0.08 to 0.2 μgL(-1) using HPLC-DAD. Also an improvement in sensitivity of several orders of magnitude was achieved using single-ion monitoring GC-MS analyses (0.04 μgL(-1)) due to compatibility of this technique with GC instrument. The applicability of the proposed HF-LLLME/GC-MS and HPLC-DAD methods was demonstrated by analyzing the drugs in spiked urine and plasma samples. The obtained recoveries of the drugs in the range of 87.9-109.2% indicated the excellent capability of the developed method for extraction of TCAs from complex matrices.
Available from: Hiroyuki Kataoka
- "ng/mg  Cocaine, morphine, 6-monoacetylmorphine Hair 100 m PDMS HS 125 • C, 25 min GC–MS 2–5 pg/mg Opiate analysis  Cocaine, cocaethylene Hair 100 m PDMS DI pH 8.5, NaCl, 25 min GC–MS 0.02–0.08 ng/mg  Cocaine, cocaethylene Plasma 100 m PDMS DI pH 9, NaCl, RT, 25 min GC–MS 11–19 ng/mL Drug abuse  Cocaine, cocaethylene Urine 100 m PDMS DI pH 8–10, RT, 20 min GC–MS 5 ng/mL Patient  Tramadol Plasma 65 m PDMS/DVB HS NaOH, 100 • C, 30 min GC–MS 0.2 ng/mL Healthy volunteers  Fentanyl Plasma PDMS, own preparation HS pH 12, 85 • C, 30 min GC–MS 0.01 ng/mL Patch treatment  Ethyl glucronide Hair 85 m CAR/PDMS HS 90 • C, 10 min GC–MS–MS 0.6 pg/mg Derivatization  Strychnine Blood 65 m CW/DVB DI Dilution (1:10 H2O), RT, 20 min GC–MS 7 ng/mL Poisoned individuals  -Tetrahydrocannabinol, cannabinol, cannabidiol Hair 100 m PDMS HS + OFD 125 • C, 20 min GC–MS 0.01 ng/mg Derivarized with BSTFA/TMCS   -Tetrahydrocannabinol, cannabinol, cannabidiol Hair 100 m PDMS HS NaOH, Na2CO3, 90 • C, 40 min GC-ITMS-MS 0.007–0.031 ng/mg THC-D3 (internal standard)  "
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ABSTRACT: Biomedical analyses of drugs, metabolites, poisons, environmental and occupational pollutants, disease biomarkers and endogenous substances in body fluids and tissues are important in the development of new drugs, therapeutic monitoring, forensic toxicology, patient diagnosis, and biomonitoring of human exposure to hazardous chemicals. In these analyses, sample preparation is essential for isolation of desired components from complex biological matrices and greatly influences their reliable and accurate determination. Solid-phase microextraction (SPME) is an effective sample preparation technique that has enabled miniaturization, automation and high-throughput performance. The use of SPME has reduced assay times, as well as the costs of solvents and disposal. This review focuses on recent advances in novel SPME techniques, including fiber SPME and in-tube SPME, in biomedical analysis. We also summarize the applications of these techniques to pharmacotherapeutic, forensic, and diagnostic studies, and to determinations of environmental and occupational exposure.
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