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1.
A method using on-line enrichment and fast high-performance liquid chromatography (HPLC) with fluorescence detection has been developed and validated for the determination of polycyclic aromatic hydrocarbons (PAHs) in atmospheric particulate samples. The evaporation step for sample preparation can be eliminated since this system allows the injection of 1000microL of sample solution. PAH recoveries were between 87% and 120% for spiked atmospheric particulate samples. The limit of detection was 0.02-0.23ng/mL (signal/noise ratio=3.3). There was good linear correlation between HPLC peak area and PAH concentration, with a linear range of 0.4-40ng/mL and correlation coefficients >0.997. Furthermore, compared to conventional approaches that include an evaporation step, the method proposed is acceptable for detecting PAHs in atmospheric particulate samples. 相似文献
2.
K. Luks-Betlej 《Chromatographia》1997,45(1):243-248
Summary Comparative results of pre-treatment methods for the extracts of polycyclic aromatic hydrocarbons (PAHs) from airborne particulate
matter for quantitative determination by gas chromatography (GC) are presented. The first method included liquid-liquid extraction
and column liquid adsorption chromatography. In the second procedure the extract was fractionated by liquid-liquid chromatography
and liquid adsorption chromatography. In the last procedure two different solid phase extraction (SPE) cartridges examined
makes it possible to separate PAHs and remove paraffinic compounds which is very important for the quantitative GC analysis
of the PAHs. Recoveries of PAH standards and some their derivatives were determined and the contents of 15 of the most important
PAHs, were compared.
Presented at the 21st ISC held in Stuttgart, Germany, 15th–20th September, 1996 相似文献
3.
Solid-Phase Extraction and LC with Fluorescence Detection for Analysis of PAHs in Rainwater 总被引:1,自引:0,他引:1
The efficiency of extraction of polycyclic aromatic hydrocarbons (PAHs) from rainwater by solid-phase extraction (SPE) with
three different types of cartridge, and analysis by high-performance liquid chromatography with fluorescence detection, are
discussed in this paper. Three cartridges were investigated but only one was suitable. After equilibration in a desiccator
for 65–80 h or in ambient air for 90–100 h the SPE cartridges were activated with 5 mL dichloromethane then 5 mL 2-propanol.
The volume of sample passed through the cartridges was 50 mL; after loading of the sample the cartridges were dried under
vacuum for approximately 20 min by application of a pressure of 15 mbar to the SPE manifold. The PAHs were eluted with 5 mL
dichloromethane–hexane, 50:50 (v/v). The flow rate used for conditioning, sample loading, and elution was 2.5 mL min−1, achieved by application of a pressure of 6 mbar. For analysis of PAHs in rainwater, recovery was between 67 and 99%, the
relative standard deviation varied between 2 and 5%, and the detection limits of the method were less than 16.9 ng L−1 for several PAHs. These optimum conditions were used for analysis of rainwater collected between June 2002 and May 2003 at
two sites in Alsace (eastern France) and 17 PAHs were quantitatively determined. Concentrations varied between 1.6 and 968.1 ng L−1. 相似文献
4.
This paper describes a simple and rapid sample preparation procedure allowing to measure the stable carbon isotopic composition of polycyclic aromatic hydrocarbons (PAHs) in petroleum and in sediments. The aromatic fraction is first purified and isolated on alumina and silica micro-columns. A high-performance liquid chromatography fractionation allows one then to isolate each aromatic family in order to limit coelutions between PAHs. Moreover, this purification step reduces the importance of the unresolved complex mixture which otherwise contribute to the GC-isotope ratio MS background signal. The application of this analytical procedure has allowed one to determined PAH isotopic composition in a reference material crude oil (SRM 1582) and a marine sediment (SRM 1944) with good reproducibility as uncertainties between three independent assays performed were lower than 0.5 per thousand. This analytical procedure has then been successfully applied to confirm the contamination of a sediment by the petroleum product spilled by the Erika tanker after its wreck on 12 December 1999 close to the Atlantic Coast of France. 相似文献
5.
《Journal of separation science》2018,41(11):2360-2367
We present a new method for simultaneous determination of 22 monoaromatic and polycyclic aromatic hydrocarbons in postoxidative effluents from the production of petroleum bitumen using dispersive liquid–liquid microextraction coupled to gas chromatography and mass spectrometry. The eight extraction parameters including the type and volume of extraction and disperser solvent, pH, salting out effect, extraction, and centrifugation time were optimized. The low detection limit ranging from 0.36 to 28 μg/L, limit of quantitation (1.1–84 μg/L), good reproducibility, and wide linear ranges, as well as the recoveries ranging from 71.74 to 114.67% revealed that the new method allows the determination of aromatic hydrocarbons at low concentration levels in industrial effluents having a very complex composition. The developed method was applied to the determination of content of mono‐ and polycyclic aromatic hydrocarbons in samples of raw postoxidative effluents in which 15 compounds were identified at concentrations ranging from 1.21 to 1017.0 μg/L as well as in effluents after chemical treatment. 相似文献
6.
Solid-phase clean-up in the liquid chromatographic determination of polycyclic aromatic hydrocarbons in edible oils 总被引:5,自引:0,他引:5
Barranco A Alonso-Salces RM Bakkali A Berrueta LA Gallo B Vicente F Sarobe M 《Journal of chromatography. A》2003,988(1):33-40
A solid-phase extraction (SPE) method for sample clean-up, followed by reversed-phase high-performance liquid chromatography (HPLC) with fluorescence detection is reported for the determination of polycyclic aromatic hydrocarbons (PAHs) in edible oils. The effects of experimental variables, such as washing and elution solvents, sample solvent and drying time have been studied using C18 cartridges. Recoveries and selectivity using other sorbent materials (C8, C2, CH, PH and NH2) were also examined, with C18 being the best one. The recoveries ranged between 50 and 103% depending on the molecular mass of the PAH. The limits of quantitation were lower than 1 ng/g for most PAHs and good precision was achieved. The method was validated using certified reference materials. 相似文献
7.
Nerea Ferreirós Bouzas Sebastian Dresen Barbara Munz Wolfgang Weinmann 《Analytical and bioanalytical chemistry》2009,395(8):2499-2507
A new quantitation method for the determination of drugs of abuse (opiates, amphetamine and derivatives, cocaine, methadone
and metabolites) in serum by using online extraction coupled to liquid chromatography (LC)–mass spectrometry (MS)/MS has been
developed. The online extraction is carried out using two extraction columns simultaneously and one analytical column. One
extraction column is loaded, while the other one is eluted by a gradient. The elution gradient also separates the analytes
in the analytical column. For the sample preparation, serum is spiked with a mixture of deuterated analogues of the drugs.
After protein precipitation with methanol/zinc sulphate, centrifugation, evaporation and reconstitution, the sample is injected
into the LC system. The quantitation is based on the analysis of two multiple reaction monitoring transitions per drug. The
recovery of the protein precipitation step is over 80% for all analytes. Intra- and interday precision, as relative standard
deviation, is lower than 6%, and in the case of accuracy, RE is lower than 15%. Only the most polar analytes showed matrix
effects. The limits of quantitation for the analysed compounds vary between 0.5 and 2.8 ng/mL. The developed method was used
to quantify basic drugs in samples “from driving under the influence of drugs” cases. The results were compared with those
obtained by using solid-phase extraction–GC–MS. 相似文献
8.
The use of electron spin resonance spectrometry with a modern instrument is described for the determination of polynuclear aromatic hydrocarbons (PAHs) down to nanogram levels, after adsorption on calcined silica/alumina. A single PAH or the total number of moles of PAHs can be determined. Implication for liquid chromatography are discussed. 相似文献
9.
色谱/质谱联用技术分析测定贻贝中的多环芳烃 总被引:5,自引:0,他引:5
介绍了GC-MS联用技术-物质征离子选择法测定贻贝中多环芳烃的分析方法,并就定性定量离子的选择,以及方法的准确度和精密度进行了探讨。结果表明,本方法适用于海洋生物贻贝,牡蛎中PAHs的分析测定。 相似文献
10.
Summary For improved determination of aromatic amines by gas chromatography and detection with an electron capture detector (GC-ECD)
a derivatization method based on the bromination of the aromatic ring in an acetic acid medium was developed. In general,
all free ortho and para-positions relative to the amino group undergo electrophilic substitution. Separation of at least 30
compounds in a single chromatographic run in 30 min is possible. With this method, 56 aromatic amines were studied and only
in 6 cases were no derivatives obtained. Quantitation limits determined from calibration data are 1.2–40 μg L−1 for a 100 mL sample and an injection volume of 1 μL. Previous experiments suggest that both sample and injection volume may
be increased to lower the quantitation limit. 相似文献
11.
Zhang J Dong X Cheng J Li J Wang Y 《Journal of the American Society for Mass Spectrometry》2011,22(7):1294-1298
In this Application Note, we describe, for the first time, the rapid analysis of hydrophobic compounds present in environmental
contaminants, which includes polycyclic aromatic hydrocarbons (PAHs) and estrogen, by matrix-assisted laser desorption/ionization
time-of-flight mass spectrometry (MALDI-TOF MS) with the use of graphene as matrix. MALDI-TOF MS with conventional matrix
has limitations in analyzing low-polarity compounds owing to their difficulty in ionization. We demonstrate that compared
with conventional matrix, graphene displays higher desorption/ionization efficiencies for PAHs, and no fragment ions are observed.
The method also holds potential in quantitative analysis. In addition, the ionization signal increases with the increasing
number of benzene rings in the PAHs, suggesting that graphene binds to PAHs via π–π stacking interactions. Furthermore, graphene
as adsorbent for solid-phase extraction of coronene from river water sample displays good performance with a detection limit
of 10–7 M. This work provides a novel and convenient method for analyzing low-polarity environmental contaminants by MALDI-TOF MS. 相似文献
12.
Trufelli H Famiglini G Termopoli V Cappiello A 《Analytical and bioanalytical chemistry》2011,400(9):2933-2941
This paper focuses on the development of a novel approach to analyze underivatized fatty acids in human plasma. The method
is based on liquid–liquid extraction followed by reversed phase liquid chromatography coupled to direct-electron ionization
mass spectrometry (LC-Direct-EI-MS). The assay is validated. Calibrations show satisfactory linearity and precision in the
investigated range of linearity. Recoveries span from 75% to 104%. The method limits of detection, varying from 0.53 to 5.35 μM,
are satisfactory for the quantitation of non-esterified fatty acids (NEFAs) in plasma at physiological levels. The method
has been successfully applied to the NEFAs profiling of plasma samples from healthy adult volunteers and subjects affected
by diabetes mellitus. Compared with published protocols based on gas chromatography–mass spectrometry and liquid chromatography
coupled to electrospray ionization mass spectrometry, this method does not require derivatization and does not show matrix
effects, thus simplifying sample preparation procedure and reducing the total time of analysis to approximately 90 min. In
addition, Direct-EI-MS allows the acquisition of high-quality NIST library-matchable EI spectra, allowing an easy-to-obtain
identification of the target NEFAs. 相似文献
13.
A method for the quantitation of polycyclic aromatic hydrocarbons (PAHs) in indoor and outdoor air by high-performance liquid chromatography (HPLC) with a spectrofluorometric detection and programmed excitation and emission wavelength pairs is proposed. The mobile phase is a linear gradient of methanol-water. The relative standard deviations (n = 5) are in the range 0.38-1.7% at concentration levels of 0.69-11.40 ng ml(-1). The determination limits (S N = 10 ) are 0.5-15.9 pg. The proposed method was successfully applied to quantitate 12 PAHs in gas phase and particulates in indoor and outdoor air. The recoveries of PAHs from gas phase and particulates were 95.7-117.5 and 94.8-112.4%, respectively. This highly sensitive automatic HPLC analysis for PAHs both in gas phase and particulates can be applied to indoor and outdoor survey. 相似文献
14.
Microwave-assisted thermal desorption (MAD) coupled to headspace solid-phase microextraction (HS-SPME) has been studied for
in-situ, one-step, sample preparation for PAHs collected on XAD-2 adsorbent, before gas chromatography with mass spectrometric
detection. The PAHs on XAD-2 were desorbed into the extraction solution, evaporated into the headspace by use of microwave
irradiation, and absorbed directly on a solid-phase microextraction fiber in the headspace. After desorption from the SPME
fiber in the hot GC injection port, PAHs were analyzed by GC–MS. Conditions affecting extraction efficiency, for example extraction
solution, addition of salt, stirring speed, SPME fiber coating, sampling temperature, microwave power and irradiation time,
and desorption conditions were investigated. Experimental results indicated that extraction of 275 mg XAD-2, containing 10–200 ng
PAHs, with 10-mL ethylene glycol–1 mol L−1 NaCl solution, 7:3, by irradiation with 120 W for 40 min (the same as the extraction time), and collection with a PDMS–DVB
fiber at 35 °C, resulted in the best extraction efficiency. Recovery was more than 80% and RSD was less than 14%. Optimum
desorption was achieved by heating at 290 °C for 5 min. Detection limits varied from 0.02 to 1.0 ng for different PAHs. A
real sample was obtained by using XAD-2 to collect smoke from indoor burning of joss sticks. The amounts of PAHs measured
varied from 0.795 to 2.53 ng. The method is a simple and rapid procedure for determination of PAHs on XAD-2 absorbent, and
is free from toxic organic solvents. 相似文献
15.
J. Hernández-Borges M. A. Rodríguez-Delgado F. J. García-Montelongo 《Chromatographia》2006,63(3-4):155-160
Several improvements in sample pretreatment for the determination of organic pollutants (i.e. n-alkanes, polycyclic aromatic hydrocarbons, PAHs) in marine biota (mussels) are presented. The use of liquid nitrogen and
homogenization of the samples are shown to be an alternative to the time consuming liophilization step required for the analysis
of biota samples. Microwave-assisted hydrolysis and extraction are combined to isolate organic pollutants (19 n-alkanes and 27 PAHs) from biota matrices. Experimental design (ED) and artificial neural networks (ANNs) were used to optimize
the experimental conditions. NIST-CRM 2978 was used to test the validity of the developed method which shows a good agreement
with certified values. 相似文献
16.
Daniele Fabbri Alessio Adamiano Cristian Torri 《Analytical and bioanalytical chemistry》2010,397(1):309-317
A method for the determination of polycyclic aromatic hydrocarbons (PAHs) in liquid pyrolysate of biomass (bio-oil) was developed
with attention to greenness along with accuracy. Bio-oil obtained from preparative pyrolysis at 500 °C of poplar wood as representative
biomass matrix was dissolved into acetonitrile (ACN). An aliquot of the ACN solution (0.1 mg bio-oil) was added with water
(20% v/v) and spiked with perdeuterated standards, then PAHs were extracted with n-hexane and separated from phenolic interferents by silica gel solid-phase extraction (SPE). All 16 priority PAHs were detected
at concentrations between 7.7 μg g−1 (naphthalene) and 0.1 μg g−1 (benz[a]anthracene) with RSD in the 6–23% range. Recovery of perdeuterated acenaphthene, phenanthrene and chrysene was 84, 93 and
90%, respectively. Results obtained from the analysis of bio-oil were used to evaluate the performance of analytical pyrolysis
conducted with a heated platinum filament in off-line configuration. Two sampling procedures were compared: (1) sorption onto
silica gel followed by elution with n-hexane (Py-SPE), (2) dynamic solid-phase micro-extraction followed by fibre cleanup with aqueous ammonia (Py-SPME). Emission
levels of priority PAHs could be determined by Py-SPE with RSD in the 13–45% range, while Py-SPME was unsatisfactory for quantitation.
Emission levels determined by Py-SPE fell in the 6.4–0.1 μg g−1 range slightly higher than those calculated from bio-oil analysis. Both Py methods were adequate for screening purposes to
assess the effect of catalysts on PAH formation. In particular, they agreed to show that the content of PAHs expected in bio-oil
increased dramatically when pyrolysis was conducted over HZSM-5 zeolite. 相似文献
17.
Spitzer T 《Analytical and bioanalytical chemistry》2008,391(8):2923-2929
Young lignite from two locations in Sendai City, Japan, were analyzed for polynuclear aromatic compounds (PACs). Lignite samples
were extracted with toluene and PACs were isolated by a compound-class-selective, reactive matrix clean-up. This clean-up
separates all compounds of polynuclear aromatic structure, for example hydrocarbons and ketones and their primary metabolites,
from interfering organic compounds. The result of this isolation procedure is, therefore, a group of a large number of polycyclic
compounds with different functional groups. Further analysis is done by glass capillary gas chromatography. Perylene was identified
as the only compound obtained by the reactive matrix clean-up of lignite samples from both locations. Concentrations were
in the range of 1–10 mg kg−1. Conversely, PACs resulting from particulate emissions from fossil fuel combustion always contain isomeric PAHs (polynuclear
aromatic hydrocarbons) with some polycyclic aromatic ketones and thousands of primary and secondary metabolites at very low
concentrations. This was demonstrated for a sample of urban air particulate matter, which is the source of PAC contamination
of surface soil. The absence of accompanying PAHs and polynuclear aromatic ketones in the lignite samples confirms that perylene
did not originate from a combustion process. It is assumed that the high concentrations of perylene are the result of a reduction
of perylene quinone. Thus, the high perylene content of the lignite samples investigated is of biogenic origin. 相似文献
18.
A modified in-tube solid phase microextraction (SPME) technique in conjunction with a high performance liquid chromatography (HPLC) was developed for the trace determination of polycyclic aromatic hydrocarbons (PAHs) in water samples. The extraction device contained a regular HPLC syringe, replacing the metallic needle by two concentric fused silica capillary tubes. The capillary tubes were coated with polydimethylsiloxane (PDMS) as the sorbent and were attached to the syringe by a homemade interface made from polyether ether ketone (PEEK). The sorption of analytes was achieved by frequent withdrawing and ejecting the water sample from/into a vial via the capillary tubes. For the desorption step, an aliquot of organic solvent was withdrawn and subsequently injected directly into the HPLC system. Limits of detection for the elected PAHs were between 0.001 and 0.006 g L–1 with a RSD of 2.6–6.3%. 相似文献
19.
Summary A detection system for gas chromatography based on gas-phase, molecular absorption measurements is presented, in which the
chromatographic column is directly joined to the spectrophotometer flow cell, without heated transfer lines. To maintain polyciclic
aromatic hydrocarbons (PAHs) in the gas phase during detection an aluminium heater was constructed. A mixture of 13 PAHs was
then separated and analyzed. Parameters affecting separation (temperature program and carrier gas flow) were studied and a
program designed to modify the measurement wavelength during the chromatography. The analytical characteristics of each compound
were calculated, obtaining detection limits 0.2–1.5 μg mL−. Given that some compounds overlaped, it was necessary to resolve their peaks mathematicaly. Finally, the method was applied
to a certified synthetic mixture, with good results. 相似文献
20.
The analysis of beta-carboline alkaloids presents a renewed interest due to their biological relevance and their increasing
popularity as recreational drugs. In the present work, a novel chromatographic reverse-phase high-performance liquid chromatography
(RP-HPLC) method with fluorimetric detection has been applied to the determination of beta-carbolines spiked in human serum
samples. The chromatographic procedure involves the use of less retentive, unusual C1 columns combined with hydro-alcoholic
mobile phases and the use of beta-cyclodextrin or (2-hydroxypropyl)-beta-cyclodextrin as mobile-phase additives. The effective
combination of C1 columns and the modified mobile phases with cyclodextrins leads to a considerable reduction in the organic
proportion in the mobile phase (up to 50%) with good resolution and efficiency. Besides, the presence of cyclodextrins allows
the use of ethanol, a green solvent, as the organic component in the mobile phase. Traditional RP-HPLC thus becomes an attractive
eco-separation technique using conventional stationary phases under simple and user-friendly experimental conditions. Solid-phase
extraction was employed as sample clean-up protocol with attractive features, i.e., a low consumption of organic solvents,
time and step economy and diminished need for sample handling. The analytical procedure was completely validated showing satisfactory
figures of merit. Limits of detection of 10−9–10−10 M can be achieved. The recoveries obtained for the total methodology (sample pre-treatment and chromatographic determination
in the case of the mobile phases containing cyclodextrins) were very satisfactory (95–107%) as well as the intraday (2–3%)
and interday precision values (3–7%). The use of 3-hydroxymethyl-beta-carboline as an internal standard allows the comparison
of the goodness of response of the analytical methodology in the presence or absence of cyclodextrins. 相似文献