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Results for “Solid Phase Microextraction”

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PubMed2003

Hollow-fibre liquid-phase microextraction of phthalate esters from water.

A simple and efficient liquid-phase microextraction (LPME) technique using a hollow-fibre membrane, in conjunction with gas chromatography-mass spectrometry has been developed for the extraction and analysis of six phthalate esters in water samples. Parameters such as extraction solvent, agitation of the sample, salt addition and extraction time were controlled and optimised. The developed protocol was found to yield a linear calibration curve in the concentration range from 0.02 to 10 microg l(-1) for most target analytes and the limits of detection were in the low microg l(-1) level, ranging between 0.005 and 0.1 microg l(-1). The repeatability of the method varied between 4% and 11%. Under the present experimental conditions, the performance of the method was found comparable to that of solid-phase microextraction (SPME). The advantage of the proposed method over SPME was that it eliminated carry-over of analytes between runs. The applicability of the developed hollow-fibre LPME method and SPME was demonstrated for real water samples. The ability of both microextraction methods to concentrate many organic analytes was demonstrated as both methods allowed the confirmation of the presence of an extra contaminant (ethyl p-ethoxybenzoate) in bottled mineral water samples.

Esters↗

PubMed2005

Use of solid-phase microextraction/gas chromatography-electron capture detection for the determination of energetic chemicals in marine samples.

Gas chromatography with electron capture detection (GC-ECD) is a highly explosive-sensitive analytical technique. However, its application to the analysis of sediment extracts is hampered by the presence of numerous endogenous interferences. In the present study, solid-phase microextraction (SPME) was used both as a purification technique for sediment extracts and as an extraction technique for water samples prior to analysis by GC-ECD. SPME/GC-ECD coupling was optimized and applied to the trace analysis of nine explosives including nitroaromatics and RDX in real seawater and marine sediment samples. Addition of a high concentration of salt (30%, w/v) in the aqueous medium and use of a carbowax/divinylbenzene (CW/DVB) coating led to optimal extraction efficiencies. Method detection limits (MDLs) ranged from 0.05 to 0.81 microg/L in water and from 1 to 9 microg/kg in dry sediment. Except for RDX, spike recoveries in seawater were satisfactory (89-147%) when samples were fortified at 2 microg/L of each analyte. Spike recoveries from dry sediment fortified at 10 microg/kg of each analyte gave lower recoveries but these could also be due to degradation in the matrix. With a smaller volume of aqueous sample required compared to solid-phase extraction (SPE), SPME is an attractive method for the analysis of limited volumes of sediment pore-water. Moreover, the use of SPME eliminated interferences present in sediment extracts thus allowing the detection of the target analytes that were otherwise difficult to detect by direct injection.

Acetonitriles↗

PubMed2005

Analysis of polycyclic aromatic hydrocarbons in wastewater treatment plant effluents using hollow fibre liquid-phase microextraction.

A simple and efficient method for the enrichment of low molecular weight polycyclic aromatic hydrocarbons (PAHs) in effluents originating from wastewater treatment plants is presented here. The proposed protocol couples the recently introduced hollow fibre liquid-phase microextraction (LPME) method with gas chromatography-mass spectrometry. Method parameters were controlled and the optimised experimental conditions were: 5 ml aqueous samples, containing 2.5% NaCl w/v, stirred at 1000 rpm, extracted with toluene for 15 min. The developed protocol yielded a linear calibration curve in the concentration range from 0.5 to 50 microg l(-1) for all target analytes (namely acenaphthene, phenanthrene, fluoranthene and pyrene) and limits of detection in the low microg l(-1) level (0.005-0.011 microg l(-1)). The repeatability and inter-day precision of the method varied between 2.7% and 11.3% and 7.9% and 14.4% respectively. The relative recoveries from different types of natural water samples revealed that matrix had a small effect on the hollow fibre LPME process. The developed method was then applied for the determination of PAHs contamination in effluent samples taken from two major municipal wastewater treatment plants. The results were compared with those obtained with solid-phase microextraction. The ability of both microextraction methods to concentrate organic analytes was demonstrated as both methods confirmed the presence of PAHs as well as of phthalates in the examined effluent samples.

Chemistry Techniques, Analytical↗

PubMed2004

Correlation between emitted and total amount of 2-cyclopentyl-cyclopentanone in polyamide 6.6 allows rapid assessment by HS and HS-SPME under non-equilibrium conditions.

A correlation was found between the emitted and total amount of 2-cyclopentyl-cyclopentanone in polyamide 6.6. The emitted amounts were measured by GC-MS after headspace (HS) or headspace solid-phase microextraction (HS-SPME) and the total content was determined after microwave-assisted extraction (MAE). The correlation was valid also under non-equilibrium conditions, which allows rapid assessment of 2-cyclopentyl-cyclopentanone content in polyamide 6.6 by headspace techniques. The incubation time needed for non-equilibrium headspace analysis could be reduced from 5 h to 45 min if the PA66 granules were milled to powder prior to extraction. However, to reach equilibrium between the analyte in the solid sample and the headspace still required 12 h of incubation at 80 degrees C. The long incubation time is explained by slow diffusion rate due to the strong hydrogen bonding between analyte and matrix and the relatively high crystallinity of polyamide 6.6. The headspace extraction profile showed several equilibrium-like patterns that are easily mistaken for the real equilibrium.

Cyclopentanes↗

PubMed2004

Determination of pesticides in soil by liquid-phase microextraction and gas chromatography-mass spectrometry.

Trace amounts of pesticides in soil were determined by liquid-phase microextraction (LPME) coupled to gas chromatography-mass spectrometry (GC-MS). The technique involved the use of a small amount (3 microl) of organic solvent impregnated in a hollow fiber membrane, which was attached to the needle of a conventional GC syringe. The organic solvent was repeatedly discharged into and withdrawn from the porous polypropylene hollow fiber by a syringe pump, with the pesticides being extracted from a 4 ml aqueous soil sample into the organic solvent within the hollow fiber. Aspects of the developed procedure such as organic solvent selection, extraction time, movement pattern of plunger, concentrations of humic acid and salt, and the proportion of organic solvent in the soil sample, were optimized. Limits of detection (LOD) were between 0.05 and 0.1 microg/g with GC-MS analysis under selected-ion monitoring (SIM). Also, this method provided good precision ranging from 6 to 13%; the relative standard deviations were lower than 10% for most target pesticides (at spiked levels of 0.5 microg/g in aqueous soil sample). Finally, the results were compared to those achieved using solid-phase microextraction (SPME). The results demonstrated that LPME was a fast (within 4 min) and accurate method to determine trace amounts of pesticides in soil.

Gas Chromatography-Mass Spectrometry↗

PubMed2002

Hollow fiber-protected liquid-phase microextraction of triazine herbicides.

A new microextraction technique termed hollow fiber-protected liquid-phase microextraction (LPME) was developed. Triazines were employed as model compounds to assess the extraction procedure and were determined by gas chromatography/mass spectrometry. Toluene functioned as both the extraction solvent and the impregnation solvent. Some important extraction parameters, such as effect of salt, agitation, pH, and exposure time were optimized. The new method provided good average enrichment factors of > 150 for eight analytes, good repeatability (RSDs <3.50%, n = 7), and good linearity (r2 > or = 0.9995) for spiked deionized water samples. The limits of detection (LODs) were in the range of 0.007-0.063 microg/L (S/N = 3) under selected ion monitoring mode. In addition to enrichment, hollow fiber-protected LPME also served as a technique for sample cleanup because of the selectivity of the membrane, which prevented large molecules and extraneous materials, such as humic acids in solution, from being extracted. The utilization of this procedure in the extraction of a slurry sample (mixture of soil and water) also gave good precision (RSDs <5.00%, n = 3) and LODs (0.04-0.18 microg/L, S/N = 3). Finally, the comparison of the new method with the static solvent drop LPME and solid-phase microextraction was performed. The results demonstrated that hollow fiber-protected LPME was a fast, accurate, and stable sample pretreatment method that gave very good enrichment factors for the extraction of triazine herbicides from aqueous or slurry samples.

Gas Chromatography-Mass Spectrometry↗

PubMed2006

Headspace solvent microextraction-gas chromatography-mass spectrometry for the analysis of volatile compounds from Foeniculum vulgare Mill.

A novel and rapid headspace solvent microextraction followed by gas chromatography-mass spectrometry (HSME-GC-MS) for the analysis of the volatile compounds of Foeniculum vulgare Mill is described. HSME parameters including extracting solvent, extraction temperature and time, headspace volume and particle size were optimized. As a result, benzyl alcohol was finally used for the extraction at 70 degrees C for 20 min with headspace volume of 12.1 ml and particle size of 120 mesh. Under the determined conditions, the powered samples of Foeniculum vulgare Mill were directly applied for the analysis. A comparison of HSME-GC-MS, solid phase microextraction (SPME)-GC-MS and steam distillation (SD)-GC-MS methods was made and showed that the HSME-GC-MS method was simple, inexpensive and effective and can be used for the analysis of volatile compounds in traditional Chinese medicines (TCMs).

Foeniculum↗

PubMed2003

A SPME-GC procedure for monitoring peppermint flavor in tablets.

A method was developed using solid-phase microextraction (SPME) and gas chromatography to monitor the peppermint flavor loss in a taste-masked tablet formulation. This was accomplished by headspace sampling of two major components of peppermint: menthone and menthol. It was found that the excipients from the tablet produced an important matrix effect and that standard addition analysis was necessary for improved accuracy of the determination. The method was shown to be specific and precise. Furthermore, the method produced acceptable results with adequate quantitation limits to determine peppermint flavors in taste-masked tablets. The optimized extraction procedure was successfully used to monitor the stability of peppermint flavor in an oral solid formulation. The accelerated stability studies of the tablet showed that the menthone and menthol was lost in an exponential manner and levels off after several days of heat exposure.

Chromatography, Gas↗

PubMed2004

Analysis of endocrine disrupting alkylphenols, chlorophenols and bisphenol-A using hollow fiber-protected liquid-phase microextraction coupled with injection port-derivatization gas chromatography-mass spectrometry.

Liquid-phase microextraction (LPME) coupled with gas chromatography-mass spectrometry were used to determine alkylphenols (APs), chlorophenols (CPs) and bisphenol-A (BPA) in aqueous samples. APs, CPs and BPA are highly polar compounds and need to be derivatized before analysis by GC-MS. In this work, they were derivatized in the GC injection port with bis(trimethylsilyl)trifluoroacetamide (BSTFA). The analytes were extracted directly from 5 ml of sample solution using 5 microl of organic solvent though a porous polypropylene hollow fiber. The hollow fiber, filled with an immiscible organic solvent (ca. 5 microl), was immersed in the sample solution which was stirred during the 30-min extraction. An aliquot (2 microl) of the extract and 2 microl of BSTFA were then consecutively injected into the GC injection port. Extraction parameters such as extraction time, pH of sample, concentration of salt added, and stirring rate were optimised. The proposed LPME provided a good average enrichment factor of up to 162-fold, reproducibility ranging from 5.9 to 13.9% (n = 4), and good linearity (r2 = 0.995) for spiked water samples. The limits of detection (LODs) ranged between 0.005 and 0.015 microgl(-1) (S/N = 3) using GC-MS with selective ion monitoring and limits of quantification were in the range of 0.012-0.026 microg l(-1). A comparative study was performed between LPME, headspace solid-phase microextraction (HS-SPME) and liquid-liquid extraction (LLE). The results obtained suggested that hollow fiber LPME was a rapid, simple and efficient technique for APs, CPs and BPA, and provided a good alternative to SPME and LLE. Finally, the proposed method was applied to monitor Singapore coastal water samples.

Endocrine Glands↗

PubMed1999

High-temperature forced-air treatment alters the quantity of flavor-related, volatile constituents present in navel and Valencia oranges.

A number of volatile compounds that contribute to orange flavor were quantified following high-temperature forced-air (HTFA) treatment of the fruit to determine if a relationship exists between the flavor loss that is observed following HTFA treatment and the volatile composition of the juice. Following different durations of HTFA treatment, fruit were stored for a period of 4 weeks and juiced and the juice subjected to headspace analysis using either a Tenax/Carbotrap column or a solid-phase microextraction device for trapping of the volatiles. alpha-Pinene, beta-myrcene, and limonene were reduced in amount by 60%, 58%, and 34%, respectively, over the course of the 5-h HTFA treatment. The influence of heat on the amount of decanal was less clear, although in one of the two fruit lots there was little change. The amount of ethanol was reduced by 70% after the initial hour of HTFA treatment and then steadily increased to exceed the initial amount during the remaining 4 h of the treatment. Taste evaluations of the fruit showed a reduction of flavor quality following 4 h or more of treatment. Percent acidity and soluble solids, two other very important determinants of flavor, were nearly unchanged by treatment. Alterations in the volatile constituents of oranges by HTFA treatment may be an important reason behind the negative impact of this treatment on flavor quality.

Beverages↗

PubMed2004

Application of single-drop microextraction to the determination of dialkyl phthalate esters in food simulants.

A fast and simple method, using static single-drop microextraction (SDME), has been developed to facilitate the identification and quantification of seven dialkyl phthalate esters in the three aqueous food simulants. The simulants were: A, distilled water; B, 3% (w/v) acetic acid/water; and C, 15% (v/v) ethanol/water. The extraction is performed by simply suspending a drop of organic solvent in the aqueous sample using a conventional gas chromatography (GC) microsyringe. Following extraction, the organic phase is withdrawn into the syringe and analyzed by gas chromatography and flame ionization detection (FID). The optimized method yields a linear calibration curve over three orders of magnitude for all the simulants, and method detection limits (MDLs) allowing detection of all the studied compounds at concentrations below migration limits established by the European Union. The accuracy of the SDME method was tested and compared to that of solid-phase microextraction (SPME) by recovery experiments using spiked samples, with results ranging from 85 to 115% in most cases.

Food Analysis↗

PubMed2005

Headspace single-drop microextraction with in-drop derivatization for aldehyde analysis.

A new technique, headspace single-drop microextraction (HS-SDME) with in-drop derivatization, was developed. Its feasibility was demonstrated by analysis of the model compounds, aldehydes in water. A hanging microliter drop of solvent containing the derivatization agent of O-2,3,4,5,6-(pentaflurobenzyl)hydroxylamine hydrochloride (PFBHA) was shown to be an excellent extraction, concentration, and derivatization medium for headspace analysis of aldehydes by GC-MS. Using the microdrop solvent with PFBHA, acetaldehyde, propanal, butanal, hexanal, and heptanal in water were headspace extracted and simultaneously derivatized. The formed oximes in the microdrop were analyzed by GC-MS. HS-SDME and in-drop derivatization parameters (extraction solvent, extraction temperature, extraction time, stirring rate microdrop volume, and the headspace volume) and the method validations (linearity, precision, detection limit, and recovery) were studied. Compared to liquid-liquid extraction and solid-phase microextraction, HS-SDME with in-drop derivatization is a simple, rapid, convenient, and inexpensive sample technique.

Journal Article↗

PubMed2006

Development of a headspace-solid phase micro extraction method to monitor changes in volatile profile of rose (Rosa hybrida, cv David Austin) petals during processing.

In the present study, headspace solid phase microextraction combined to capillary gas chromatography (HS-SPME-GC) has been applied for the determination of changes in the volatile profile of rose petals (Rosa hybrida, cvs David Austin) following processing (heat treatment and addition as an ingredient to a food product--for example yoghurt). Four SPME fibres at two sampling temperatures (40 and 60 degrees C) with a sampling time of 30 min were examined. Volatile profiles were detected either by FID or/and by olfactometry (ODP-II, Gerstel). Fibre testing was performed using raw rose petals for sampling temperature selection and an 18 characteristic rose volatile standard mixture in water was used to compare fibre performances at the sampling temperature of 60 degrees C. Polydimethylsiloxane-divinylbenzene (PDMS-DVB) fibre at the sampling temperature of 60 degrees C was the most suitable to sample the rose alcohols phenyl ethanol, citronellol, nerol, geraniol and eugenol, as assessed by GC-olfactometry, not only from raw petals, but also from processed rose petals and the food product. PDMS-DVB fibre also showed a desired low affinity to volatiles from yoghurt, which reduces the influence of food matrix on the volatile profile. The method was linear over two orders of magnitude and had satisfactory repeatability, with limits of detection for the rose alcohols ranging from <1 to 10 ng/ml concentration levels.

Chromatography, Gas↗

PubMed2006

Dispersive liquid-liquid microextraction combined with gas chromatography-flame photometric detection. Very simple, rapid and sensitive method for the determination of organophosphorus pesticides in water.

A new method was used for the extraction of organophosphorus pesticides (OPPs) from water samples: dispersive liquid-liquid microextraction (DLLME) coupled with gas chromatography-flame photometric detection (GC-FPD). In this extraction method, a mixture of 12.0 microL chlorobenzene (extraction solvent) and 1.00 mL acetone (disperser solvent) is rapidly injected into the 5.00 mL water sample by syringe. Thereby, a cloudy solution is formed. In fact, the cloudy state is because of the formation of fine droplets of chlorobenzene, which has been dispersed among the sample solution. In this step, the OPPs in water sample are extracted into the fine droplets of chlorobenzene. After centrifuging (2 min at 5000 rpm), the fine droplets of chlorobenzene are sedimented in the bottom of the conical test tube (5.0+/-0.3 microL). Sedimented phase (0.50 microl) is injected into the GC for separation and determination of OPPs. Some important parameters, such as kind of extraction and disperser solvent and volume of them, extraction time, temperature and salt effect were investigated. Under the optimum conditions, the enrichment factors and extraction recoveries were high and ranged between 789-1070 and 78.9-107%, respectively. The linear range was wide (10-100,000 pg/mL, four orders of magnitude) and limit of detections were very low and were between 3 to 20 pg/mL for most of the analytes. The relative standard deviations (RSDs) for 2.00 microg/L of OPPs in water with internal standard were in the range of 1.2-5.6% (n=5) and without internal standard were in the range of 4.6-6.5%. The relative recoveries of OPPs from river, well and farm water at spiking levels of 50, 500 and 5000 pg/mL were 84-125, 88-123 and 93-118%, respectively. The performance of proposed method was compared with solid-phase microextraction (SPME) and single drop microextraction. DLLME is a very simple and rapid (less than 3 min) method, which requires low volume of sample (5 mL). It also has high enrichment factor and recoveries for extraction of OPPs from water.

Chromatography, Gas↗

PubMed2005

Sol-gel approach to in situ creation of high pH-resistant surface-bonded organic-inorganic hybrid zirconia coating for capillary microextraction (in-tube SPME).

A novel zirconia-based hybrid organic-inorganic sol-gel coating was developed for capillary microextraction (CME) (in-tube SPME). High degree of chemical inertness inherent in zirconia makes it very difficult to covalently bind a suitable organic ligand to its surface. In the present work, this problem was addressed from a sol-gel chemistry point of view. Principles of sol-gel chemistry were employed to chemically bind a hydroxy-terminated silicone polymer (polydimethyldiphenylsiloxane, PDMDPS) to a sol-gel zirconia network in the course of its evolution from a highly reactive alkoxide precursor undergoing controlled hydrolytic polycondensation reactions. A fused silica capillary was filled with a properly designed sol solution to allow for the sol-gel reactions to take place within the capillary for a predetermined period of time (typically 15-30 min). In the course of this process, a layer of the evolving hybrid organic-inorganic sol-gel polymer got chemically anchored to the silanol groups on the capillary inner walls via condensation reaction. At the end of this in-capillary residence time, the unbonded part of the sol solution was expelled from the capillary under helium pressure, leaving behind a chemically bonded sol-gel zirconia-PDMDPS coating on the inner walls. Polycyclic aromatic hydrocarbons, ketones, and aldehydes were efficiently extracted and preconcentrated from dilute aqueous samples using sol-gel zirconia-PDMDPS coated capillaries followed by thermal desorption and GC analysis of the extracted solutes. The newly developed sol-gel hybrid zirconia coatings demonstrated excellent pH stability, and retained the extraction characteristics intact even after continuous rinsing with a 0.1 M NaOH solution for 24 h. To our knowledge, this is the first report on the use of a sol-gel zirconia-based hybrid organic-inorganic coating as an extraction medium in solid phase microextraction (SPME).

Chromatography, Gas↗

PubMed1997

Rapid determination of corticosteroids in urine by combined solid phase microextraction/liquid chromatography/mass spectrometry.

Solid-phase microextraction combined with fast short-column liquid chromatography/mass spectrometry (SPME/LC/MS) was used for isolating and analysing 11 corticosteroids and 2 steroid conjugates from urine samples. Several SPME parameters such as polarity of fibres, extraction time and effect of ionic strength, were investigated, and their impact on the SPME/LC/MS technique was studied. To demonstrate the potential of the SPME/LC/MS method, its application to the determination of steroids in human urine was investigated. The method was shown to be sensitive with detection limits between 4 and 30 ng/mL and precision between 4.9 and 11.1% RSD through the use of an internal standard technique. The versatility of the method was also exhibited by its excellent linearity in the concentration range of 20 to 20,000 ng/mL in urine for all investigated compounds. A comparison of the SPME/LC/MS method with LC/MS methods utilizing traditional sample preparation techniques, shows that the former offers similar performance in terms of precision, linearity and detection limits, but is clearly easier to use and faster to perform.

Adrenal Cortex Hormones↗

PubMed1998

Study of erythromycin A decomposition products in aqueous solution by solid-phase microextraction/liquid chromatography/tandem mass spectrometry.

The decomposition of erythromycin A (EA) in aqueous solution was examined in the pH range 2-13 by means of combined solid-phase microextraction (SPME) and liquid chromatography/electrospray ionization tandem mass spectrometry. Degradation of EA, especially at lower pH values (pH < or = 3), was very rapid and yielded a wide variety of decomposition products. Identification of these degradation products was achieved by means of tandem mass spectrometry in the product ion and precursor ion scan modes. Anhydroerythromycin A was shown to be the major reaction product in both acidic and basic solutions. Among the different SPME fibers investigated for extraction from aqueous solutions, polydimethylsiloxane/divinylbenzene exhibited the best performance for EA and its degradation products.

Chromatography, Thin Layer↗

PubMed1999

Rapid analysis of tetracycline antibiotics by combined solid phase microextraction/high performance liquid chromatography/mass spectrometry.

The technique of solid phase microextraction (SPME) combined on-line with high performance liquid chromatography/mass spectrometry (HPLC/MS) has been applied to the analysis of seven tetracycline analogues. Rapid baseline separation was achieved in under 5 min using a short 3 microm RP-18e cartridge column. Optimisation of the SPME procedure is described including choice of extracting fibre and modification of the sample by heating or salting out of the analytes. Detection limits of 4-40 ng/mL were obtained for the various analogues from extracted aqueous samples and absolute amounts of analyte extracted by the method determined using external calibration. To demonstrate the applicability of the technique for real samples the extraction of tetracycline from milk is described.

Animals↗