Development of a simple in-vial liquid-phase microextraction device for drug analysis compatible with capillary gas chromatography, capillary electrophoresis and high-performance liquid chromatography

Rasmussen, Knut; Pedersen‐Bjergaard, Stig; Krogh, Mette; Ugland, Hege Grefslie; Grønhaug, Trine

doi:10.1016/s0021-9673(99)01163-2

Cited by 291 publications

(126 citation statements)

References 21 publications

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“…To extract acidic analytes, the pH of the donor aqueous solution must be adjusted in the acidic range so as to deionise the target compounds, reduce their solubility within the sample solution and ensure efficient transfer into the organic phase which is impregnated in the pores of the hollow fiber. 29,30 In order to transfer the analytes into the acceptor phase through the organic phase without back-extraction into the donor phase, the pH of the acceptor phase have to be adjusted into the basic range. This results in ionization of target analytes (acidic compounds) and ensures higher solubility of target compounds in the acceptor phase than into the organic phase.…”

Section: Resultsmentioning

confidence: 99%

Determination of Non-Steroidal Anti-Inflammatory Drugs in Human Urine Sample using HPLC/UV and Three Phase Hollow Fiber-Liquid Phase Microextraction (HF-LPME)

Byoung¹,

Myung

2013

Bulletin of the Korean Chemical Society

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Three phase hollow fiber-liquid phase microextraction (HF-LPME), which is faster, simpler and uses a more environmentally friendly sample-preparation technique, was developed for the analysis of Non-Steroidal AntiInflammatory Drugs (NSAIDs) in human urine. For the effective simultaneous extraction/concentration of NSAIDs by three phase HF-LPME, parameters (such as extraction organic solvent, pH of donor/acceptor phase, stirring speed, salting-out effect, sample temperature, and extraction time) which influence the extraction efficiency were optimized. NSAIDs were extracted and concentrated from 4 mL of aqueous solution at pH 3 (donor phase) into dihexyl ether immobilized in the wall pores of a porous hollow fiber, and then extracted into the acceptor phase at pH 13 located in the lumen of the hollow fiber. After the extraction, 5 µL of the acceptor phase was directly injected into the HPLC/UV system. Simultaneous chromatographic separation of seven NSAIDs was achieved on an Eclipse XDB-C18 (4.6 mm i.d. × 150 mm length, 5 µm particle size) column using isocratic elution with 0.1% formic acid and methanol (30:70) at a HPLC-UV/Vis system. Under optimized conditions (extraction solvent, dihexyl ether; pH donor , 3; pH acceptor , 13; stirring speed, 1500 rpm; NaCl salt, 10%; sample temperature, 60 o C; and extraction time, 45 min), enrichment factors (EF) were between 59 and 260. The limit of detection (LOD) and limit of quantitation (LOQ) in the spiked urine matrix were in the concentration range of 5-15 ng/mL and 15-45 ng/mL, respectively. The relative recovery and precision obtained were between 58 and 136% and below 15.7% RSD, respectively. The calibration curve was linear within the range of 0.015-0.96 ng/mL with the square of the correlation coefficient being more than 0.997. The established method can be used to analyse of NSAIDs of low concentration (ng/mL) in urine.

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Section: Resultsmentioning

confidence: 99%

Determination of Non-Steroidal Anti-Inflammatory Drugs in Human Urine Sample using HPLC/UV and Three Phase Hollow Fiber-Liquid Phase Microextraction (HF-LPME)

Byoung¹,

Myung

2013

Bulletin of the Korean Chemical Society

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“…The difference in pH between the donor and acceptor phases can promote the extracted analyte from donor to acceptor phase [1,16,18,[22][23][24]. Scopolamine is a moderately basic drug (pK b = 7.75) and the pH of the aqueous sample should be higher than the pKa of the analyte, so that the analyte is neutral and extractable into the organic phase and contrary for acceptor phase.…”

Section: Ph Of the Donor And Acceptor Phasesmentioning

confidence: 99%

“…However, the volume of the acceptor solution used for extraction may also be adjusted depending on the analytical technique coupled to liquid phase microextraction. For example, in contrast to GC, sample volumes in the range from 10 to 25 µL are easily injected into a HPLC instrument, so the whole acceptor phase may be analyzed, potentially providing lower detection limits [24]. In this manner, the use of a large drop results in an increase of the analytical response.…”

Section: Phase Volumementioning

confidence: 99%

Liquid Chromatographic Determination of Scopolamine in Hair with Suspended Drop Liquid Phase Microextraction Technique

Masrournia¹,

haghi²,

Amini³

2011

AJAC

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Hair analysis is used in some branches of alternative medicine as a method of investigation to assist diagnosis. It is very useful when a history of drug use is difficult or impossible to obtain. In this research suspended droplet liquid phase microextraction (SDLME) coupled with high-performance liquid chromatography and photodiode array detection (HPLC-DAD) was used for preconcentration and analysis of scopolamine in hair samples. Therefore scopolamine was extracted from 2.0 g hair sample incubated in methanol (5 h, 50˚C) and adjusted to pH 7.4 with, Na 2 HPO 4 -H 3 PO 4 buffer solution (donor phase, P 1 ) into an organic phase (P 2 ) 350 µl n-octanol and then back extracted into a micro drop of aqueous acceptor phase (P 3 ), adjusted at pH 3, with HCL. The extraction time, T 1 (from P 1 to P 2 ) was 2 min and T 2 (from P 2 to P 3 ) was 30 min. Optimum instrumental conditions were included; A C 18 reverse phase column with water-acetonitrilemethanol (80:10:10) as the mobile phase was used and wavelength for UV detection was 205 nm. The linear range was 10 to 10000 ng·mL -1 , enrichment factor, detection limit and relative standard deviation were 77, 0.1 ng·mL -1 and 5.4 respectively.

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“…Following this procedure the acceptor solution could be analyzed by HPLC or capillary electrophoresis (CE), without further treatment. It has been proven that HF-LPME is very useful for extraction of drugs and metabolites from biological matrices and pollutants from environmental samples with simultaneous clean-up of the matrices [25][26][27][28].…”

Section: Introductionmentioning

confidence: 99%

Trace Determination of Tamoxifen in Biological Fluids Using Hollow Fiber Liquid-Phase Microextraction Followed by High-Performance Liquid Chromatography-Ultraviolet Detection

Kashtiaray¹,

Farahani²,

Farhadi³

et al. 2011

AJAC

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The applicability of hollow fiber liquid-phase microextraction (HF-LPME) combined with high-performance liquid chromatography-ultraviolet detection (HPLC-UV) was evaluated for the extraction and determination of tamoxifen (TAM) in biological fluids including human urine and plasma. The drug was extracted from a 15 mL aqueous sample (source phase; SP) into an organic phase impregnated in the pores of the hollow fiber (membrane phase; MP) followed by the back-extraction into a second aqueous solution (receiving phase; RP) located in the lumen of the hollow fiber. The effects of several factors such as the nature of organic solvent, compositions of SP and RP solutions, extraction time, ionic strength and stirring rate on the extraction efficiency were examined and optimized. An enrichment factor of 360 along with substantial sample clean up was obtained under the optimized conditions. The calibration curve showed linearity in the range of 1 -500 ng·mL -1 and the limit of detection was found to be 0.5 ng·mL -1 in aqueous medium. A reasonable relative recovery (≥89%) and satisfactory intra-assay (3.7% -4.2%, n = 3) and inter-assay (7.5% -7.8%, n = 3) precision illustrated good performance of the analytical procedure in spiked human urine and plasma samples.

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Development of a simple in-vial liquid-phase microextraction device for drug analysis compatible with capillary gas chromatography, capillary electrophoresis and high-performance liquid chromatography

Cited by 291 publications

References 21 publications

Determination of Non-Steroidal Anti-Inflammatory Drugs in Human Urine Sample using HPLC/UV and Three Phase Hollow Fiber-Liquid Phase Microextraction (HF-LPME)

Determination of Non-Steroidal Anti-Inflammatory Drugs in Human Urine Sample using HPLC/UV and Three Phase Hollow Fiber-Liquid Phase Microextraction (HF-LPME)

Liquid Chromatographic Determination of Scopolamine in Hair with Suspended Drop Liquid Phase Microextraction Technique

Trace Determination of Tamoxifen in Biological Fluids Using Hollow Fiber Liquid-Phase Microextraction Followed by High-Performance Liquid Chromatography-Ultraviolet Detection

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