[Determination of diamorphine metabolites in urine by solid phase microextraction coupled with GC/MS].
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Gas Chromatography-Mass Spectrometry↗
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Results for “Solid Phase Microextraction”
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[Determination of residual acetone in soybean phospholipids by headspace solid-phase microextraction and gas chromatography].
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Acetone↗
[Method for analyzing urinary organic solvents by solid-phase microextraction (SPME) for biological monitoring of exposure to these solvents].
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Chromatography, Gas↗
Sample preparation for gas chromatography with solid-phase extraction and solid-phase microextraction.
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Chromatography, Gas↗
Determination of parabens in pharmaceutical formulations by solid-phase microextraction-ion mobility spectrometry.
Solid-phase microextraction (SPME) coupled with ion mobility spectrometry (IMS) was used for the detection and quantitation of 4-hydroxybenzoate preservatives, methylparaben, ethylparaben, propylparaben, and butylparaben, in commercial pharmaceutical products. For the first time, SPME-IMS is described for the simultaneous detection, separation, and quantitation of multiple analytes in complex matrixes. The parabens are extracted from the samples using SPME, and the analytes on the fiber are heated by the IMS desorber unit and vaporized into the drift tube. The four preservatives differing only by a methyl group were separated in less than 18 ms. The analytical procedure was optimized for fiber coating selection, extraction time, sample pH, sample volume, ionic strength, and IMS conditions. Separation characteristics such as resolution, theoretical plates, and drift times of the parabens were also evaluated based on the direct interfacing of SPME to IMS. The conditions were tested using six over-the-counter topical products containing various combinations of preservatives. Analysis of the samples by SPME-IMS using benzyl paraben as an internal standard yields good comparison to an HPLC method, thereby reinforcing the applicability of this technique as a method for routine analysis. Limits of detection were 10 ng/mL for methylparaben and ethylparaben and 5 ng/mL for propylparaben and butylparaben. Good linearity range and reproducibility of less than 8% were obtained.
Calibration↗
[Determination of phthalic diesters in water by solid phase microextraction-capillary gas chromatography].
The solid phase microextraction (SPME) has the advantages of high efficiency, high sensitivity, simple operation and solvent free operation for analyzing environmental samples. An optical fiber coated with mixed stationary phase of polysiloxane and polymeric fullerene (in ratio of 4:1) was used to extract 5 phthalic diesters by HS-SPME-GC. The operating conditions of SPME such as the extraction temperature, ionic strength of solution, adsorption time and desorption time have been studied. It was compared with commercial polymer coating PDMS fiber through headspace SPME combined with GC. The results indicated that OV-1/PSO-C60 was better than PDMS in extracting high boiling point and semi-volatile phthalic diesters. For phthalic diesters, the detection limits were in the range of 0.331 ng/L-12.5 micrograms/L, and relative standard deviations were below 12% except for dinonyl phthalate.
Chromatography, Gas↗
Determination of terpenes in tequila by solid phase microextraction-gas chromatography-mass spectrometry.
Solid phase microextraction and capillary gas chromatography-mass spectrometry were used for the determination of seven terpenes in tequila. The method was selected based on the following parameters: coating selection (PA, PDMS, CW/DVB, and PDMS/DVB), extraction temperature, addition of salt, and extraction time profile. The extraction conditions were: PDMS/DVB fiber, Headspace, 100% NaCl, 25 degrees C extraction temperature, 30 min extraction time and stirring at 1200 rpm. The calibration curves (50-1000 ng/ml) for the terpenes followed linear relationships with correlation coefficients (r) greater than 0.99, except for trans,trans-farnesol (r = 0.98). RSD values were smaller than 10% confirmed that the technique was precise. Samples from 18 different trade brands of "Aged" tequila analyzed with the developed method showed the same terpenes in different concentrations. The analytical procedure used is selective, robust (more than 100 analyses with the same fiber), fast and of low-cost.
Alcoholic Beverages↗
Evaluation of exudates by solid phase microextraction-gas chromatography.
Head-space solid phase microextraction combined with gas chromatography (SPME-GC) was used for the determination of bacterial volatile fatty acid (VFA) patterns. The method was validated with cultures of reference bacterial strains. It was confirmed that VFA production depends on the composition of the cultivation medium, which limits accurate characterisation of particular bacterial species. A set of 195 clinical exudates of various origin and consistence was analysed using SPME-GC and compared with 73 samples extracted using tert-butyl methyl ether. Approximate agreement of VFA profiles with cultivation findings was found in most cases. However, 20.5% of clinical exudates with distinct VFA profiles appeared to be false-negative by cultivation. Using SPME-GC of exudates, the frequency of false-negative cultivations was higher than that of solvent extraction of exudates or blood cultures found previously. The described method is suitable for preliminary detection of bacteria, particularly non-sporulating anaerobes, in clinical samples. It can reveal false-negative findings due to cultivation. Analysis can be performed in 30 min without the need for cultivation.
Bacteria, Anaerobic↗
[Determination of volatile organic compounds in blood by headspace solid-phase microextraction-gas chromatography].
The headspace solid-phase microextraction (HS-SPME) is a novel extraction technique and has been developed rapidly. It is a fast, simple, solventless and sensitive method for sampling, separating, extracting, injecting and analyzing volatile organic compounds. This paper presents the research work in detecting volatile organic compounds(including ten compounds) in blood. The extraction fiber is made by fused-silica fiber with 100 microns polydimethylsiloxane (PDMS). The extraction time of the method was 10 min. The thermal desorption time was 1 min. It was found that the optimized location of the extraction fiber in the injector of GC was to put the whole needle in the injector. The precision of the method was determined to be less 5% relative standard deviation (RSD). The linear range of the detection was rather wide. The lowest detectin limits (LODs) were all < or = 5 ng/ml.
Animals↗
Quantitative determination of formaldehyde in cosmetics using a combined solid-phase microextraction-isotope dilution mass spectrometry method.
Solid-phase microextraction (SPME) in conjunction with isotope dilution mass spectrometry (ID-MS) was employed for the analysis of formaldehyde in cosmetic products. The formaldehyde is derivatized in situ with pentafluorophenyl hydrazine. The formed hydrazone is adsorbed over a poly(dimethylsiloxane)-divinylbenzene-coated fiber and analyzed using gas chromatography-mass spectrometry. The adsorption-time profiles and salting effect were studied. The quantitation was performed by using a stable isotope labeled analogue as an internal standard. The precision, recovery and detection limits were determined with spiked samples. The relative standard deviations from different spiked cosmetic samples were all less than 10% and the recoveries were between 89.00 and 101.23%. The limit of detection was of 0.39 microg/l. Compared with other techniques, the study shown here provides a simple, fast and reliable method for the analysis of formaldehyde in cosmetic products.
Calibration↗
Determination of microcystins in cyanobacterial blooms by solid-phase microextraction-high-performance liquid chromatography.
A solid-phase microextraction (SPME) method was applied to study microcystin (MC) profiles in a natural Microcystis sp. bloom in a freshwater pond in Guangzhou, China. Three dominant MC variants, namely MC-LR, MC-YR, and MC-RR, were quantified. Simultaneous study of their total, extracellular, and intracellular profiles was made possible using SPME coupled to high-performance liquid chromatography. The total and intracellular concentrations of MC-LR in the bloom were 8.67 x 10(-2) microg/ ml and 1.93 mg/g, respectively. The corresponding concentrations of MC-YR were 1.20 x 10(-3) microg/ml and 0.06 mg/g, respectively, and those of MC-RR were 5.57 x 10(-2) microg/ml and 1.49 mg/g, respectively. Only MC-LR was detectable in the extracellular phase (1.49 x 10(-2) microg/ml) of the bloom, and its concentration was 14% of the intracellular content. Mass balance consideration revealed that only 71.1% of total MC-LR, 36.0% of total MC-YR, and 67.4% of total MC-RR within the cyanobacterial cells were released into the aqueous phase immediately after cell lysis.
Chromatography, High Pressure Liquid↗
Flavour analysis of Greek white wine by solid-phase microextraction-capillary gas chromatography-mass spectrometry.
Solid-phase microextraction (SPME) was optimised for the qualitative determination of the volatile flavour compounds responsible for the aroma of Greek Boutari wine. Several factors influencing the equilibrium of the aroma compounds between the sample and the SPME fiber were taken into account, including the extraction time, the extraction temperature, the sampling mode (headspace and direct immersion or liquid SPME), and the presence of salt. Four different SPME fibers were used in this study. namely poly(dimethylsiloxane) (PDMS), poly(acrylate), carbowax-divinylbenzene and divinylbenzene-carboxen on poly(dimethylsiloxane). The best results were obtained using the PDMS fiber during headspace extraction at 25 degrees C for 30 min after saturating the samples with salt. The optimised SPME method was then applied to investigate the qualitative aroma composition of three other Greek wines, namely Zitsa, Limnos and Filoni.
Flavoring Agents↗
Helical sorbent for fast sorption and desorption in solid-phase microextraction-gas chromatographic analysis.
A new technique for solid-phase microextraction (SPME) of analytes using a helical solid sorbent followed by thermal desorption into a gas chromatographic injector is reported. The main factors that affect the mass transport of analytes in sorption and thermal desorption process using a poly(dimethylsiloxane) (PDMS) helical sorbent are described. The sorption and thermal desorption were achieved in a few seconds, being very close by the theoretical prediction. Both processes were very fast by the reduction of the thickness of boundary layer between sorbent and gaseous sample as a result of a turbulent rotational flow of the headspace air on the surface of sorbent, which is generated by the helical configuration of the sorbent. The thermal desorption was also reduced by improving heat transfer into a thin boundary layer and by increasing the temperature of the heat transporter (carrier gas). The sorption and desorption with PDMS helical sorbent were compared with those of the PDMS silica rod. The extraction time was as much as 15 times faster with the PDMS helical sorbent than with the PDMS silica rod. The desorption with the PDMS helical sorbent was very fast, giving narrow peaks without tailing and a high efficiency of separation in comparison with PDMS silica rod.
Chemistry Techniques, Analytical↗
Experimental design to optimise the analysis of organic volatile compounds in cow slurry by headspace solid-phase microextraction-gas chromatography-mass spectrometry.
The headspace solid-phase microextraction (HS-SPME) of some odorous organic compounds [volatile fatty acids (VFAs), phenols and indoles] from animal wastes was optimised using an experimental design approach. The variables affecting the HS-SPME process studied were as follows: type of fibre, pH of the slurry (3-7), addition of sodium chloride (0-1 mol L(-1)), sample volume (10-30 mL), exposure time (10-30 min), exposure temperature (25-50 degrees C), desorption time (3-10 min) and desorption temperature (230-310 degrees C). As for the sorbent, three different types of fibres were studied: 50/30 microm divinylbenzene/Carboxen/polydimethylsiloxane (DVB/CAR/PDMS), 100 microm PDMS and 85 microm CAR/PDMS. Methylation VFAs was observed when fibres containing PDMS were used. The analytes studied in the optimisation procedure were acetic acid, propanoic acid, butanoic acid, 3-methylbutanoic acid, pentanoic acid, phenol, 4-methylphenol, 4-ethylphenol, indole and skatole (3-methylindole). In order to study the influence of the variables on the responses of the compounds, a Plackett-Burman design was built using the Unscrambler program. The optimisation was carried out using real samples. In order to take into account the matrix effect on the calibration curves, standard solutions were prepared using a purged cow slurry free from the analytes of interest. Repeatability within and among days, accuracy and detection limits were calculated from these calibration curves.
Animals↗
Screening of Brazilian fruit aromas using solid-phase microextraction-gas chromatography-mass spectrometry.
Manual headspace solid-phase microextraction (SPME) coupled to gas chromatography-mass spectrometry (GC-MS) was used for the qualitative analysis of the aromas of four native Brazilian fruits: cupuassu (Theobroma grandiflorum, Spreng.), cajá (Spondias lutea. L.), siriguela (Spondias purpurea, L.) and graviola (Anona reticulata, L). Industrialized pulps of these fruits were used as samples, and extractions with SPME fibers coated with polydimethylsiloxane, polyacrylate, Carbowax and Carboxen were carried out. The analytes identified included several alcohols, esters, carbonyl compounds and terpernoids. The highest amounts extracted, evaluated from the sum of peak areas, were achieved using the Carboxen fiber.
Fruit↗
Influence of fibre coating in headspace solid-phase microextraction-gas chromatographic analysis of aromatic and medicinal plants.
Solid-phase microextraction (SPME) is a solvent-free technique, which is well established in headspace analysis since it is sensitive, because of the concentration factor achieved by the fibres, and selective, because of different coating materials which can be used. The performance of eight commercially available SPME fibres was compared to evaluate the recoveries of some characteristic components with different polarities and structures present in the headspace of four aromatic and medicinal plants: rosemary (Rosmarinus officinalis L.), sage (Salvia officinalis L.), thyme (Thymus vulgaris L.) and valerian (Valeriana officinalis L.). The relative concentration capacity of each fibre on the same components of each plant was also determined by comparing their abundance with that obtained by classical static-headspace GC. The partition coefficient, K1, between the headspace gaseous phase and SPME polymeric coating, and the relative concentration factors, of some of the characteristic components of the plant investigated dissolved in dibutyl phtalate, were also determined, under rigorously standardised analysis conditions. The results showed that the most effective fibres were those consisting of two components, i.e., a liquid phase (polydimethylsiloxane) and a porous solid (carboxen or divinylbenzene, or both).
Chromatography, Gas↗
Vapor-phase analysis of isobutyl acetate, isopropyl acetate, n-propyl acetate and their respective alcohols using solid-phase microextraction-gas chromatography with a mass selective detector.
A solid-phase microextraction (SPME)-GC-MS method for three esters and the corresponding alcohols was tested for responses in accuracy, within-run precision (repeatability), and between-run precision (reproducibility) due to individual operators, individual analysis days, and differing analyte concentrations. At 5 ppm (v/v) [ppmv], three of the six analytes showed significant (p < 0.05) operator effects, while five of six analytes gave a significant effect due to the days of analysis. At 20 ppmv, five of the six analytes gave significant operator and daily effects. At 100 ppmv, all the analytes showed significant daily effects but no operator effects were observed. The repeatability was concentration dependent, with all six analytes combining for an average RSD of 12.1 +/- 6.1% at 1 ppmv, becoming most precise at 50 ppmv at 1.01 +/- 0.45%, then increasing at 100 ppmv to 4.12 +/- 1.88%. The contributors to error trended as: concentration > daily effects > operator.
2-Propanol↗
Determination of amphetamine and methamphetamine in serum via headspace derivatization solid-phase microextraction-gas chromatography-mass spectrometry.
This study evaluates solid-phase microextraction (SPME) coupled with gas chromatography-mass spectrometry (GC-MS) to determine trace levels of amphetamine and methamphetamine in serum. Headspace post-derivatization in a laboratory-made design with heptafluorobutyric anhydride vapor following SPME was compared with that without derivatization SPME. The SPME experimental procedures to extract amphetamine and methamphetamine in serum were optimized with a relatively non-polar poly(dimethylsiloxane) coated fiber at pH 9.5, extraction time for 40 min and desorption at 260 degrees C for 2 min. Experimental results indicate that the concentration of the serum matrix diluted to a quarter of original (1:3) ratio by using one volume of buffer solution of boric acid mixed with sodium hydroxide and two volumes of water improves the extraction efficiency. Headspace derivatization following SPME was performed by using 6 microl 20% (v/v) heptafluorobutyric anhydride ethyl acetate solution at an oil bath temperature of 270 degrees C for 10 s. The precision was below 7% for analysis for without derivatization and below 17% for headspace derivatization. Detection limits were obtained at the ng/l level, one order better obtained in headspace derivatization than those achieved without derivatization. The feasibility of applying the methods to determine amphetamine and methamphetamine in real samples was examined by analyzing serum samples from methamphetamine abused suspects. Concentrations of the amphetamine and methamphetamine ranged from 6.0 microg/l (amphetamine) to 77 microg/l (methamphetamine) in serum.
Amphetamines↗