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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- "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. "
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.Journal of Chromatography A 12/2011; 1222:5-12. DOI:10.1016/j.chroma.2011.11.055 · 4.26 Impact Factor
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- "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)  "
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.Journal of pharmaceutical and biomedical analysis 04/2011; 54(5):926-50. DOI:10.1016/j.jpba.2010.12.010 · 2.83 Impact Factor
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- "Plasma / serum HS - SPME PDMS / DVB ( 60 ) GC Sha et al . , 2005"
ABSTRACT: This paper reviews the recent developments in bioanalysis sample preparation techniques and gives an update on basic principles, theory, applications and possibilities for automation, and a comparative discussion on the advantages and limitation of each technique. Conventional liquid-liquid extraction (LLE), protein precipitation (PP) and solid-phase extraction (SPE) techniques are now been considered as methods of the past. The last decade has witnessed a rapid development of novel sample preparation techniques in bioanalysis. Developments in SPE techniques such as selective sorbents and in the overall approach to SPE, such as hybrid SPE and molecularly imprinted polymer SPE, have been addressed. Considerable literature has been published in the area of solid-phase micro-extraction and its different versions, e.g. stir bar sorptive extraction, and their application in the development of selective and sensitive bioanalytical methods. Techniques such as dispersive solid-phase extraction, disposable pipette extraction and micro-extraction by packed sorbent offer a variety of extraction phases and provide unique advantages to bioanalytical methods. On-line SPE utilizing column-switching techniques is rapidly gaining acceptance in bioanalytical applications. PP sample preparation techniques such as PP filter plates/tubes offer many advantages like removal of phospholipids and proteins in plasma/serum. Newer approaches to conventional LLE techniques (salting-out LLE) are also covered in this review article.Biomedical Chromatography 02/2011; 25(1-2):199-217. DOI:10.1002/bmc.1560 · 1.66 Impact Factor