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PubMed2006

Application of comprehensive two-dimensional gas chromatography for the assessment of oil contaminated soils.

A crucial step in the remediation of oil contaminated soils is the characterization of the pollution. Information on the chemical composition is used to assess the toxicity (and thus the need for remediation) and to determine the most appropriate technology for treatment. Mostly these analyses are carried out in routine environmental laboratories using gas chromatography with flame ionization detection (GC/FID) based on a protocol developed by the Total Petroleum Hydrocarbon Criteria Working Group (TPHCWG). In the present study, an alternative method was developed using comprehensive two-dimensional gas chromatography (GCXGC) with FID. Sample preparation was limited to pressurized liquid extraction (PLE), and the analysis was carried out on a commercially available instrument with a conventional column combination (RTX-1/BPX50) and with standard chromatographic software. Compared to the TPH method, the group-types in the GCXGC analysis are chemically better defined and more specific information is obtained especially for the (toxicologically important) aromatic hydrocarbon fraction. Preliminary results indicate that higher recoveries and lower RSDs are obtained with GCXGC, probably because of the less complex sample preparation. Furthermore a data processing method was developed to generate TPH results from GCXGC data; the volatility distribution profiles compared very well with conventional TPH data. The possibility of extracting physicochemical properties directly from the GCXGC chromatogram was briefly explored, but software limitations hindered this promising application.

Analytic Sample Preparation Methods↗
PubMed1997

[Study on the direct determination of Pb and Cd in milk powder by GFAAS].

The paper reports the direct determination of Pb and Cd in milk powder by GFAAS. The mothed does not need any pre-treatment to the samples and fully use some function of pre-treatment which the Graphite Furnace have. The result indicates that the method is simple, rapid and accurate, and the false result from any pre-treatment to the samples can be reduced. The recover rate of Pb is 100.1%, CV =2.7 ; and Cd is 98.6%, CV = 3.1 %. This method is also applied to the rapid determination of Pb and Cd in soluble samples with satisfactory results.

Analytic Sample Preparation Methods↗
PubMed2006

Determination of zearalenone and its metabolites in urine, plasma and faeces of horses by HPLC-APCI-MS.

The paper describes a method for the sensitive and selective determination of zearalenone and its metabolites in urine, plasma and faeces of horses by high performance liquid chromatography and atmospheric pressure chemical ionisation (APCI) mass spectrometry (MS). While only one step sample clean-up by an immunoaffinity column (IAC) was sufficient for plasma samples, urine and faeces samples had to be prepared by a combination of a solid-phase extraction (SPE) and an immunoaffinity column. The method allows the simultaneous determination of zearalenone and all of its metabolites; alpha-zearalenol, beta-zearalenol, alpha-zearalanol, beta-zearalanol and zearalanone. Dideuterated zearalanone was used as internal standard for quantification and the study of the matrix effect. Recovery rates between 56 and slightly above 100% were achieved in urine samples, and more than 80% in plasma and faeces samples. The limits of detection ranged from 0.1-0.5 microg/l or microg/kg, the limits of quantification from 0.5-1.0 microg/l or microg/kg. The practical use of the method is demonstrated by the analysis of spiked and naturally contaminated urine, plasma and faeces of horses.

Analytic Sample Preparation Methods↗
PubMed2006

Determination of antihyperglycemic biguanides in serum and urine using an ion-pair solid-phase extraction technique followed by HPLC-UV on a pentafluorophenylpropyl column and on an octadecyl column.

An HPLC-UV method was established for the determination of metformin and buformin in biological fluids. Metformin was not retained on particles packed in conventional solid-phase extraction cartridges; in contrast, buformin was retained too firmly and not eluted with a solvent for recovery. However, both drugs were retained on particles that had been treated with an ion-pair reagent of heptanesulfonate or dodecylsulfate and recovered almost completely. The recovered fraction was subjected to HPLC on a pentafluorophenylpropyl column which was suitable for the determination of both biguanides in serum and in urine. Limits of quantitation were low enough for clinical use, and reproducibility was high with an RSD of 0.9-2.3%. HPLC on a conventional octadecyl column was suitable only for the determination of buformin in serum since interfering peaks appeared on the chromatograms of urine samples. The method was applied to analysis of some clinical specimens.

Alkanes↗
PubMed1997

[Simultaneous determination of 16 elements in decoction solution of Chinese herbal medicine by ICP-AES].

A new method has been developed for simultaneous derermination of 16 elements in decoction solution of Chinese herbal medicine by ICP-AES after pretreatrment the solution with HNO3-H2O2. This method has low and stable blank value. The detection limits of 0.1-5ng/ml for most elements and recoveries of 85-103% were obtained. This method has been applied to the determination of 16 elements in decoction solution of chinese herbal medicine with satisfactory reswls.

Analytic Sample Preparation Methods↗
PubMed1999

[Gas chromatographic method for the analysis of polychlorinated biphenyls in pine needles].

Polychlorinated biphenyls (PCBs) are a class of 209 chemical compounds, in which 1-10 chlorine atoms are attached to a biphenyl molecule. PCBs are members of halogenated aromatic group of environmental pollutants that have been identified worldwide in diverse environmental matrices. PCBs in air, soils, sediment, water, transformer oils and other environmental matrices have been determined in the past years. In this work a method for routine analysis of PCBs in pine needles has been developed. First, extractions were carried out in Soxhlet apparatus with n-hexane as solvent. Then, a silica gel chromatographic column was applied to pretreat the pine needle samples. The reference standard used was clophen 50. The recovery was about 90%, so the feasibility and reliability were assured. After the analysis of PCBs in pine needle samples from four different regions, the distribution of PCBs in environment can be discussed and monitored. In this method, a Shimadzu GC-7A gas chromatograph equipped with a 63Ni electron capture detector was used for the analysis of PCBs. From the results, we can see the PCB pollution in different regions. So evaluation of air pollution level through foliage data is feasible. The sample preparation and analytical method mentioned in this paper is reliable and simple.

Chromatography, Gas↗
PubMed2006

Recent developments in methods and technology for analysis of biological samples by MALDI-TOF-MS.

Matrix-assisted laser desorption/ionization-time-of-flight mass spectrometry (MALDI-TOF-MS) is widely used in a variety of fields because it has the characteristics of speed, ease of use, high sensitivity, and wide detectable mass range for obtaining molecular weights and for structural characterization of macromolecules. In this article we summarize recent developments in matrix additives, new matrices, and sample-pretreatment methods using off-probe or on-probe techniques or nanomaterials for MALDI-TOF-MS analysis of biological samples.

Analytic Sample Preparation Methods↗
PubMed2006

On-line derivatization gas chromatography with furan chemical ionization tandem mass spectrometry for screening of amphetamines in urine.

A simple alternative method with minimal sample pretreatment is investigated for screening of amphetamines in small volume (using only 20 microL) of urine sample. The method is sensitive and selective. The method uses gas chromatography (GC) direct sample introduction (DSI) for on-line derivatization (acylation) of amphetamines to improve sensitivity. Furan as chemical ionization (CI) reagent in conjunction with tandem mass spectrometry (MS/MS) is used to improve selectivity. Low background with sharp protonated molecular ion peaks of analytes is the evidence of improvement in sensitivity and selectivity. Blank urine samples spiked with known amounts of amphetamine, methamphetamine, 3,4-methylenedioxyamphetamine, 3,4-methylenedioxymethamphetamine and 3,4-methylenedioxyethylamphetamine is analyzed. Selected ion monitoring of the characteristic product ions (m/z 119+136+150+163) using furan CI-MS/MS in positive ion mode is used for quantification. Limits of detection (LOD) between 0.4 and 1.0 ng mL(-1) and limits of quantitation (LOQ) between 1.0 and 2.0 ng mL(-1) are established. Linear response over the range of 1-1000 ng mL(-1) (r(2)>0.997) is observed for all analytes, except for methamphetamine (2.0-1000 ng mL(-1)). Good accuracy between 86 and 113% and precision ranging from 4 to 18% is obtained. The method is also tested on real samples of urine from suspected drug abusers. This method could be used for screening and determination of amphetamines in urine samples, however needs additional work for full validation.

Amphetamines↗
PubMed2006

On-line strategies for determining trace levels of nitroaromatic explosives and related compounds in water.

We report the development and tests of several systems for the simultaneous determination of 18 energetic compounds and related congeners in untreated water samples. In these systems a Restricted Access Material trap or liquid-chromatography precolumn (with a C(18) or porous graphitic carbon, PGC, stationary phase) followed by a PGC analytical column are used for sample clean-up, enrichment and separation of the trace level analytes, which are then analyzed by mass spectrometry (MS). The relative merits of two MS ionization interfaces (atmospheric pressure chemical ionization, APCI, and atmospheric pressure photoionization, APPI) were also compared for the MS identification and quantification of these analytes. APCI was found to be superior in cases where both alternatives are applicable. A major drawback when applying APPI is that no signal is obtained for the cyclic nitramines and nitrate esters. Using APCI, a wide spectrum of unstable compounds can be determined in a single analysis, and the feasibility of using large volume samples (up to 100 mL) in combination with the sensitivity of the MS detection system provide method detection limits ranging from 2.5 pg/mL (for 2,4-dinitrotoluene and 2,6-diamino-6-nitrotoluene) to 563 pg/mL (for pentaerythritol tetranitrate, PETN), with repeatability ranging from 2 to 7%. Other chemometric parameters such as robustness, selectivity, repeatability, and intermediate precision were also evaluated in the validation of the extraction methods for use in water analysis. Tests with untreated groundwater and drinking water samples, spiked with 20 ng of the analytes, yielded results similar to those obtained with high purity water samples.

Analytic Sample Preparation Methods↗
PubMed1997

[Extraction-flame atom absorption determination of trace copper, zinc, cadmium and iron in bones].

Trace content of Cu, Zn, Cd and Fe in bones is determined by flame atomic absorption spectrometry after preceding preconcentration using the extraction system O-phenanthroline-sodium perchlorate/1, 2-dichloroethane. Also, the factors of influence were studied. The method was simple, accurate and reliable, The detection limits were Cu: 0.038microg/ml, Zn: 0.0042microg/ml, Cd: 0.0019microg/ml, Fe: 0.02microg/ml. The recovery rate was between 92.8 and 105%.

Analytic Sample Preparation Methods↗
PubMed2006

Development of gas chromatography-mass spectrometry following microwave distillation and simultaneous headspace single-drop microextraction for fast determination of volatile fraction in Chinese herb.

In this work, for the first time, microwave distillation (MD) coupled with simultaneous headspace single-drop microextraction (HS-SDME) was developed for the determination of the volatile components in the Chinese herb, Artemisia capillaris Thunb. The volatile components were rapidly isolated by MD, and simultaneously extracted and concentrated by using a dodecane microdrop. The volatile oil extracted in the microdrop solvent was analyzed by gas chromatography-mass spectrometry (GC-MS). The experimental parameters of solvent selection, microdrop volume, microwave power, irradiation time and sample amount were investigated, and the method precision was also studied. The optimal parameters were extraction solvent of dodecane, solvent volume of 2.0 microL, microwave power of 400 W, irradiation time of 4 min, and sample amount of 2.0 g. Thirty-five volatile compounds present in Artemisia capillaris Thunb. were identified by using the proposed method, which were identical with those obtained by the conventional steam distillation method. The experimental results showed that MD-HS-SDME is a simple, rapid, reliable, and solvent-free technique for the determination of volatile compounds in Chinese herbs.

Analytic Sample Preparation Methods↗
PubMed2006

Development of a simple hollow fibre supported liquid membrane extraction method to extract and preconcentrate dinitrophenols in environmental samples at ng L(-1) level by liquid chromatography.

An easy and rapid hollow-fibre supported liquid membrane method (HFSLM) has been developed to extract and determinate the total concentration of four dinitrophenols in environmental water at ng L(-1) level. This extraction method provides a high selectivity, short extraction time and very low cost for real samples. It is a three-phase system, aqueous-organic-aqueous, where the organic solvent is held into the fibre pores, being in contact with the two other phases. The organic phase is formed by two different organic solvents, with two different polarities, n-undecane and toluene (1:1). The optimization step was performed using a three-variable Doehler design, involving three factors, stirring speed, fibre length and sample volume. The organic phase composition, as well as the pH of the acceptor and donor phases was also optimized. The extraction equilibrium was reached after 30 min, after which essentially the total amount (90-80%) of the four dinitrophenolic compounds were extracted from the sample. Better repeatability and reproducibility at the expense of lower enrichment factors was obtained compared with other methods, employing incomplete extraction during a fixed time. The matrix effect was tested by performing extractions from leachate water and river water. This method is linear in the range 0.1-100 microgL(-1) in different matrices, with detection limit around 100 ng L(-1), after extraction of 6 mL of sample and using high performance liquid chromatography for final analysis.

Analytic Sample Preparation Methods↗
PubMed1998

[Determination of total Ca in the lung tissue of rats by FAAS].

Determination of total Ca in the Lung Tissue of Rats by FAAS was described, with a mixed microemulsion consisting of sodium dodecyl sulfate, N-dodecyl, N-dimethyl benzol ammonium bromide and nonyl phenol polyethyeneoxy ether. Comparing the result of the microemulsion FAAS with that of solution FAAS showed that the former was better than the latter in sensitivity, precision, selectivity and linearity of the calibration curve, with a detection limit of 1.92 microg x cm(-3), relative standard deviation of 1.92% (n = 10) and linear regressive coefficient of 0.9998 of the calibration curve over 0-20 microg x cm(-3) calcium. The method was applied to determine calcium amount in the lung tissue of rats, and the results were in accordance with those odtained by the conventional solution FAAS, in which a sample was reduced to ashes at a high temperature.

Analytic Sample Preparation Methods↗
PubMed2006

Determination of polybrominated diphenyl ethers in domestic dust by microwave-assisted solvent extraction and gas chromatography-tandem mass spectrometry.

In this paper, a rapid and simple method for the analysis of polybrominated diphenyl ethers (PBDEs) in house dust samples based on microwave-assisted solvent extraction (MASE) and gas chromatography-tandem mass spectrometry (GC-MS/MS) is presented. Extraction conditions were optimized using a multifactorial experimental design approach. The use of an aqueous NaOH phase in combination with a non-polar organic phase (hexane) to extract the target analytes from dust allowed an efficient extraction and reduced chromatographic background. The final hexane extracts could be analyzed after a simple one-step cleanup procedure using Florisil. The validation of the method was performed in terms of accuracy, linearity, and repeatability. The limits of detection (LODs) ranged from 0.29 to 0.55 ng/g for all compounds. The target PBDEs were found in several real dust samples collected in urban and rural houses of Northwestern Spain.

Analytic Sample Preparation Methods↗
PubMed2006

Site-specific sampling of taurine from rat brain followed by on-line sample pre-concentration, throughout in-capillary derivatization and capillary electrophoresis.

A method of pinpoint-sampling followed by on-line pre-concentration of the sample, throughout in-capillary derivatization and capillary electrophoretic separation was evaluated by demonstrating the detection of taurine, 2-aminoethanesulfonic acid at a specific location of a rat brain. The direct sampling of taurine from the rat brain was accomplished by using voltage injection associated with two kinds of driving forces, electrophoretic flow and electroosmotic flow (EOF). The capillary tube (75 microm of inner diameter x 375 microm of outer diameter) of the capillary electrophoresis (CE) apparatus was already filled with a CE run buffer, viz., 40 mM phosphate-borate buffer (pH 10) containing 2mM o-phthalaldehyde (OPA)/N-acetylcysteine (NAC) as the derivatization reagent. One end of a platinum wire (0.5mm o.d.), used as the anode, and the inlet end of capillary tube (from which a 1.0 cm long polyimide coating was removed), were pricked down onto the surface of either the cerebrum or cerebellum of a rat brain at a location of very small dimension. When a low voltage (5 kV, 30s) was applied, taurine began to move from the rat brain into the capillary tube, and, simultaneously, electric focusing of taurine occurred by the action of "the pH-junction effect" at the inlet end of the capillary tube. After completing the injection, both the platinum wire and capillary tube were detached from the brain and dipped into the run buffer in an anode reservoir filed with the same solution as that in the capillary tube for the CE apparatus. Then, by applying a high voltage (20 kV) between the ends of the capillary tube, taurine was automatically derivatized to yield the fluorescent derivative, separated and detected with fluorescence (E(x)=340 nm, E(m)=455 nm) during migration throughout the capillary tube. The migration profiles obtained from cerebrum and cerebellum appeared to be different, but the peak corresponding to taurine was identified on both electropherograms. The efficacy of the present method including sample on-line pre-concentration prior to throughout in-capillary derivatization CE was first verified with several preliminary experiments by using samples of taurine in water, saline and a piece of 1.5% agar-gel block, as an alternate standard for the rat brain used in this study.

Analytic Sample Preparation Methods↗