共查询到20条相似文献,搜索用时 93 毫秒
1.
Ru-Song Zhao Xia Wang Jing Sun Shan-Shan Wang Jin-Peng Yuan Xi-Kui Wang 《Analytical and bioanalytical chemistry》2010,397(4):1627-1633
A novel and environmentally friendly microextraction method, termed ionic liquid dispersive liquid-phase microextraction (IL-DLPME),
has been developed for rapid enrichment of triclosan and triclocarban before analysis by high-performance liquid phase chromatography–electrospray
tandem mass spectrometry (HPLC–ESI-MS–MS). Instead of using toxic organic solvents, an ionic liquid was used as a green extraction
solvent. This also avoided the instability of the suspending drop in single-drop liquid-phase microextraction, and the heating
and cooling step in temperature-controlled ionic liquid dispersive liquid phase microextraction. Factors that may affect the
enrichment efficiency, for example volume of ionic liquid, type and volume of dispersive solvent, pH, extraction time, and
NaCl content were investigated in detail and optimized. Under optimum conditions, linearity of the method was observed over
the range 0.2–12 μg L−1 for triclocarban and 1–60 μg L−1 for triclosan with correlation coefficients ranging from 0.9980 to 0.9990, respectively. The sensitivity of the proposed
method was found to be excellent, with limits of detection in the range 0.040–0.58 μg L−1 and precision in the range 7.0–8.8% (RSD, n = 5). This method has been successfully used to analyze real environmental water samples and satisfactory results were achieved.
Average recoveries of spiked compounds were in the range 70.0–103.5%. All these results indicated that the developed method
would be a green method for rapid determination of triclosan and triclocarban at trace levels in environmental water samples. 相似文献
2.
A simple and efficient method, based on ultrasound-enhanced surfactant-assisted dispersive liquid–liquid microextraction (UESA-DLLME)
followed by high-performance liquid chromatography (HPLC) has been developed for extraction and determination of ketoconazole
and econazole nitrate in human blood samples. In this method, a common cationic surfactant, cetyltrimethylammonium bromide
(CTAB), was used as dispersant. Chloroform (40 μL) as extraction solvent was added rapidly to 5 mL blood containing 0.068 mg mL−1 CTAB. The mixture was then sonicated for 2 min to disperse the organic chloroform phase. After the extraction procedure,
the mixture was centrifuged to sediment the organic chloroform phase, which was collected for HPLC analysis. Several conditions,
including type and volume of extraction solvent, type and concentration of the surfactant, ultrasound time, extraction temperature,
pH, and ionic strength were studied and optimized. Under the optimum conditions, linear calibration curves were obtained in
the ranges 4–5000 μg L−1 for ketoconazole and 8–5000 μg L−1 for econazole nitrate, with linear correlation coefficients for both >0.99. The limits of detection (LODs, S/N = 3) and enrichment factors (EFs) were 1.1 and 2.3 μg L−1, and 129 and 140 for ketoconazole and econazole nitrate, respectively. Reproducibility and recovery were good. The method
was successfully applied to the determination of ketoconazole and econazole nitrate in human blood samples. 相似文献
3.
Zang X Wang J Wang O Wang M Ma J Xi G Wang Z 《Analytical and bioanalytical chemistry》2008,392(4):749-754
A novel method was developed for the determination of captan, folpet, and captafol in apples by dispersive liquid–liquid microextraction
(DLLME) coupled with gas chromatography–electron capture detection (GC–ECD). Some experimental parameters that influence the
extraction efficiency, such as the type and volume of the disperser solvents and extraction solvents, extraction time, and
addition of salt, were studied and optimized to obtain the best extraction results. Under the optimum conditions, high enrichment
factors for the compounds were achieved ranging from 824 to 912. The recoveries of fungicides in apples at spiking levels
of 20.0 μg kg−1 and 70.0 μg kg−1 were 93.0–109.5% and 95.4–107.7%, respectively. The relative standard deviations (RSDs) for the apple samples at 30.0 μg kg−1 of each fungicide were in the range from 3.8 to 4.9%. The limits of detection were between 3.0 and 8.0 μg kg−1. The linearity of the method ranged from 10 to 100 μg kg−1 for the three fungicides, with correlation coefficients (r
2) varying from 0.9982 to 0.9997. The obtained results show that the DLLME combined with GC–ECD can satisfy the requirements
for the determination of fungicides in apple samples.
Figure Dispersive liquid–liquid microextraction (DLLME) coupled with gas chromatography–electron capture detection (GC–ECD) allows
satisfactory determination of fungicides in apple samples 相似文献
4.
Ionic liquids are a kind of environmentally friendly solvents which have drawn great attention in many fields. The potential
of ionic liquid as dispersive liquid-phase microextraction (DLPME) solvent for the enrichment of typical persistent organic
pollutants, dichlorodiphenyltrichloroethane (DDT), and its metabolites including 1,1-dichloro-2,2-bis-(4′-chlorophenyl)ethane
and 1,1-dichloro-2,2-bis-(4′-chlorophenyl)ethylene has been investigated. Parameters that may influence the extraction efficiency,
such as the type and volume of ionic liquid, the type and volume of disperser solvent, extraction time, and sample pH, were
investigated and optimized in detail. The experimental results showed the excellent linear relationship between peak area
and the concentration of DDT and its metabolites over the range of 1–50 μg L−1, and the precisions (RSDs) were 5.27–6.73% under the optimal conditions. The limits of detection could reach 0.33–0.63 μg L−1. Satisfied results were achieved when the proposed method was applied to determine the target compounds in real-world water
samples with spiked recoveries over the range 94.4–115.3%. All these facts indicated that ionic liquid DLPME coupled to HPLC
was an environmentally friendly alternative for the rapid analysis of DDT and its metabolites at trace level in environmental
water samples. 相似文献
5.
Zhao RS Diao CP Wang X Jiang T Yuan JP 《Analytical and bioanalytical chemistry》2008,391(8):2915-2921
This paper describes a novel, simple and environmentally friendly method for rapid determination of the amide herbicides metoalchlor,
acetochlor, and butachlor. It is based on dispersive liquid-liquid microextraction and gas chromatography–mass spectrometry.
Factors that may influence the enrichment efficiency, such as type and volume of extraction solvent, type and volume of dispersive
solvent, extraction time, and content of NaCl, were investigated and optimized in detail. Under the optimum conditions, the
limits of detection of metoalchlor, acetochlor, and butachlor were 0.02, 0.04, and 0.003 μg L−1, respectively. The experimental results indicated that there was linearity over the range 0.1–50 μg L−1 and good reproducibility with relative standard deviations over the range 1.6–3.0% (n = 5). The proposed method has been applied for the analysis of real-world water samples, and satisfactory results were achieved.
Average recoveries of spiked herbicides were in the range 80.3–108.8%. All of these indicated that the developed method would
be an efficient method for simultaneous determination of the three herbicides in environmental water samples. 相似文献
6.
Zhou Y Han L Cheng J Guo F Zhi X Hu H Chen G 《Analytical and bioanalytical chemistry》2011,399(5):1901-1906
A method for analysis of diethofencarb and pyrimethanil in apple pulp and peel was developed by using dispersive liquid–liquid
microextraction based on solidification of a floating organic droplet (DLLME-SFO) and high-performance liquid chromatography
with diode-array detection (HPLC–DAD). Acetonitrile was used as the solvent to extract the two fungicides from apple pulp
and peel, assisted by microwave irradiation. When the extraction process was finished, the target analytes in the extraction
solvent were rapidly transferred from the acetonitrile extract to another extraction solvent (1-undecanol) by using DLLME-SFO.
Because of the lower density of 1-undecanol than that of water, the finely dispersed droplets of 1-undecanol collected on
the top of aqueous sample and solidified at low temperature. Meanwhile, the tiny particles of apple cooled and precipitated.
Recovery was tested for a concentration of 8 μg kg−1. Recovery of diethofencarb and pyrimethanil from apple pulp and peel was in the range 83.5–101.3%. The repeatability of the
method, expressed as relative standard deviation, varied between 4.8 and 8.3% (n = 6). Detection limits of the method for apple pulp and peel varied from 1.2–1.6 μg kg−1 for the two fungicides. Compared with conventional sample preparation, the method has the advantage of rapid speed and simple
operation, and has high enrichment factors and low consumption of organic solvent. 相似文献
7.
A novel microextraction method is introduced based on dispersive liquid–liquid microextraction (DLLME) in which an in situ
metathesis reaction forms a water-immiscible ionic liquid (IL) that preconcentrates aromatic compounds from water followed
by separation using high-performance liquid chromatography. The simultaneous extraction and metathesis reaction forming the
IL-based extraction phase greatly decreases the extraction time as well as provides higher enrichment factors compared to
traditional IL DLLME and direct immersion single-drop microextraction methods. The effects of various experimental parameters
including type of extraction solvent, extraction and centrifugation times, volume of the sample solution, extraction IL and
exchanging reagent, and addition of organic solvent and salt were investigated and optimized for the extraction of 13 aromatic
compounds. The limits of detection for seven polycyclic aromatic hydrocarbons varied from 0.02 to 0.3 μg L−1. The method reproducibility produced relative standard deviation values ranging from 3.7% to 6.9%. Four real water samples
including tap water, well water, creek water, and river water were analyzed and yielded recoveries ranging from 84% to 115%.
相似文献
8.
Directly suspended droplet liquid–liquid–liquid microextraction (LLLME) has been used to determine residues of diclofenac
(2-[2-(2,6-dichlorophenyl) aminophenyl] ethanoic acid), in environmental water samples. In this technique a free suspended
droplet of an aqueous solvent is delivered to the top-center position of an immiscible organic solvent floating on the top
of an aqueous sample while being agitated by a stirring bar placed on the bottom of the sample cell. Recently, diclofenac
was found as an environmental contaminant in sewage, surface, ground and drinking water samples. In the present work, diclofenac
was extracted from water samples by LLLME and analysed by HPLC with UV detection at 281 nm. Factors such as organic solvent,
extraction and back extraction times, stirring rate and the pH of acceptor and donor phases were optimized. Enrichment factor
and detection limit (LOD, n = 7) were 102 and 0.1 μg L−1, respectively. The linearity ranged from 0.5 to 2,000 μg−1 with a %RSD (n = 5) of 7.2 at S/N = 3. All experiments were carried out at room temperature (22 ± 0.5 °C). 相似文献
9.
R. Rahnama Kozani Y. Assadi F. Shemirani M. R. Milani Hosseini M. R. Jamali 《Chromatographia》2007,66(1-2):81-86
Dispersive liquid–liquid microextraction (DLLME) has been used for preconcentration of trihalomethanes (THMs) in drinking
water. In DLLME an appropriate mixture of an extraction solvent (20.0 μL carbon disulfide) and a disperser solvent (0.50 mL
acetone) was used to form a cloudy solution from a 5.00-mL aqueous sample containing the analytes. After phase separation
by centrifugation the enriched analytes in the settled phase (6.5 ± 0.3 μL) were determined by gas chromatography with electron-capture
detection (GC–ECD). Different experimental conditions, for example type and volume of extraction solvent, type and volume
of disperser solvent, extraction time, and use of salt, were investigated. After optimization of the conditions the enrichment
factor ranged from 116 to 355 and the limit of detection from 0.005 to 0.040 μg L−1. The linear range was 0.01–50 μg L−1 (more than three orders of magnitude). Relative standard deviations (RSDs) for 2.00 μg L−1 THMs in water, with internal standard, were in the range 1.3–5.9% (n = 5); without internal standard they were in the range 3.7–8.6% (n = 5). The method was successfully used for extraction and determination of THMs in drinking water. The results showed that
total concentrations of THMs in drinking water from two areas of Tehran, Iran, were approximately 10.9 and 14.1 μg L−1. Relative recoveries from samples of drinking water spiked at levels of 2.00 and 5.00 μg L−1 were 95.0–107.8 and 92.2–100.9%, respectively. Comparison of this method with other methods indicates DLLME is a very simple
and rapid (less than 2 min) method which requires a small volume of sample (5 mL). 相似文献
10.
Chunxia Wu Huimin Liu Weihua Liu Qiuhua Wu Chun Wang Zhi Wang 《Analytical and bioanalytical chemistry》2010,397(6):2543-2549
A simple dispersive liquid–liquid microextraction based on solidification of floating organic droplet coupled with high-performance
liquid chromatography–diode array detection was developed for the determination of five organophosphorus pesticides (OPs)
in water samples. In this method, the extraction solvent used is of low density, low toxicity, and proper melting point near
room temperature. The extractant droplet could be collected easily by solidifying it in the lower temperature. Some important
experimental parameters that affect the extraction efficiencies were optimized. Under the optimum conditions, the calibration
curve was linear in the concentration range from 1 to 200 ng mL−1 for the five OPs (triazophos, parathion, diazinon, phoxim, and parathion-methyl), with the correlation coefficients (r) varying from 0.9991 to 0.9998. High enrichment factors were achieved ranging from 215 to 557. The limits of detection were
in the range between 0.1 and 0.3 ng mL−1. The recoveries of the target analytes from water samples at spiking levels of 5.0 and 50.0 ng mL−1 were 82.2–98.8% and 83.6–104.0%, respectively. The relative standard deviations fell in the range of 4.4% to 6.3%. The method
was suitable for the determination of the OPs in real water samples. 相似文献
11.
Dispersive liquid-liquid microextraction and liquid chromatographic determination of pentachlorophenol in water 总被引:1,自引:0,他引:1
Khalil Farhadi Mir A. Farajzadeh Amir A. Matin Paria Hashemi 《Central European Journal of Chemistry》2009,7(3):369-374
A simple and sensitive dispersive liquid-liquid microextraction method for extraction and preconcentration of pentachlorophenol
(PCP) in water samples is presented. After adjusting the sample pH to 3, extraction was performed in the presence of 1% W/V
sodium chloride by injecting 1 mL acetone as disperser solvent containing 15 μL tetrachloroethylene as extraction solvent.
The proposed DLLME method was followed by HPLC-DAD for determination of PCP. It has good linearity (0.994) with wide linear
dynamic range (0.1–1000 μg L−1) and low detection limit (0.03 μg L−1), which makes it suitable for determination of PCP in water samples.
相似文献
12.
Arroyo-Manzanares N García-Campaña AM Gámiz-Gracia L 《Analytical and bioanalytical chemistry》2011,401(9):2987-2994
Ochratoxin A (OTA) is a mycotoxin naturally found in various foods, including wine. As OTA is considered as a possible human
carcinogen, the maximum concentration for this compound has been established at 2 μg kg−1 in wine by the EU (Directive (CE) No 1881/2006). Typically, immunoaffinity columns have been used for its extraction. However,
simpler, more efficient and less contaminant extraction systems are demanding. In this work, dispersive liquid–liquid microextraction
using ionic liquid as extractant solvent (IL-DLLME) and the QuEChERS procedure, have been evaluated and compared for extraction
of OTA in wine samples. Laser-induced fluorescence (LIF, He–Cd Laser excitation at 325 nm) coupled with capillary HPLC has
been used for the determination of OTA, using a sodium dodecyl sulfate micellar solution in the mobile phase to increase the
fluorescence intensity. Matrix-matched calibration curves were established for both methods, obtaining LODs (3× S/N) of 5.2 ng·L−1 and 85.7 ng·L−1 for IL-DLLME and QuEChERS, respectively. Clean extracts were obtained for white, rose and red wines with both methods, with
recoveries between 88.7–94.2% for IL-DLLME and between 82.6–86.2% for QuEChERS. The precision was evaluated in terms of repeatability
(n = 9) and intermediate precision (n = 15), being ≤ 8.5% for IL-DLLME and ≤ 5.4% for QuEChERS. 相似文献
13.
A novel method for the determination of five sulfonylurea herbicides in soil was developed by a dispersive solid-phase extraction
(DSPE) clean-up followed by dispersive liquid–liquid microextraction (DLLME), prior to sweeping micellar electrokinetic chromatography
(MEKC). In the DSPE-DLLME, 10 g of soil sample was first extracted with 10 mL of acetonitrile containing 5% formic acid (pH 3.0).
The extract was then cleaned-up by a DSPE with C18 as sorbent. A 1 mL aliquot of the resulting extract was then added into a centrifuge tube containing 5 mL of water adjusted
to pH 2.0 and 60.0 μL chlorobenzene (as extraction solvent) for DLLME procedure. Then, the organic sample extraction solution
was evaporated to dryness, and reconstituted with 20.0 μL of 1.0 mmol L−1 Na2HPO4 (pH 10.0) for sweeping-MEKC analysis after DLLME. Under optimized conditions, the method provided as high as 3,000- to 5,000-fold
enrichments factors. The linearity of the method was in the range of 3.3–200 ng g−1 for chlorimuron ethyl and bensulfuron methyl, and in the range of 1.7–200 ng g−1 for tribenuron methyl, chlorsulfuron and metsulfuron methyl, with the correlation coefficients (r) ranging from 0.9965 to 0.9983, respectively. The limits of detection (LODs) ranged from 0.5 to 1.0 ng g−1. The intraday relative standard deviations (RSDs, n = 5) were below 5.3% and interday RSDs (n = 15) within 6.8%. The recoveries of the method for the five sulfonylureas from soil samples at spiking levels of 5.0, 20.0,
and 100.0 ng g−1 were 76.0–93.5%, respectively. The developed method has been successfully applied to the analysis of the target sulfonylurea
herbicide residues in soil samples with a satisfactory result. 相似文献
14.
N. Negreira I. Rodríguez E. Rubí R. Cela 《Analytical and bioanalytical chemistry》2010,398(2):995-1004
The performance of the dispersive liquid–liquid microextraction (DLLME) technique for the determination of eight UV filters
and a structurally related personal care species, benzyl salicylate (BzS), in environmental water samples is evaluated. After
extraction, analytes were determined by gas chromatography combined with mass spectrometry detection (GC-MS). Parameters potentially
affecting the performance of the sample preparation method (sample pH, ionic strength, type and volume of dispersant and extractant
solvents) were systematically investigated using both multi- and univariant optimization strategies. Under final working conditions,
analytes were extracted from 10 mL water samples by addition of 1 mL of acetone (dispersant) containing 60 μL of chlorobenzene
(extractant), without modifying either the pH or the ionic strength of the sample. Limits of quantification (LOQs) between
2 and 14 ng L−1, inter-day variability (evaluated with relative standard deviations, RSDs) from 9% to 14% and good linearity up to concentrations
of 10,000 ng L−1 were obtained. Moreover, the efficiency of the extraction was scarcely affected by the type of water sample. With the only
exception of 2-ethylhexyl-p-dimethylaminobenzoate (EHPABA), compounds were found in environmental water samples at concentrations between 6 ± 1 ng L−1 and 26 ± 2 ng mL−1. 相似文献
15.
D. Leyva J. Estévez A. Montero I. Pupo 《Journal of Radioanalytical and Nuclear Chemistry》2012,291(3):699-705
A sensitive and non chromatographic analytical procedure for the separation of inorganic selenium species in natural water
has been performed. A combination of APDC coprecipitation and determination by an absolute thin layer Energy dispersive X-ray
fluorescence spectrometry method was used. The influence of various analytical parameters such as element concentration, oxidation
states and pH on the recoveries of Se (IV) was examined. The presence of organic matter and bicarbonate anions, typical components
in Cuban groundwater samples, was also tested. Negligible matrix effects were observed. At pH 4 a 100% recovery was found
for Se (IV). The coprecipitation recovery of the oxidized selenium species (Se (VI)) was null for the selected concentration
range (5–100 μg L−1). When the Se (VI) was reduced by heating the solution with 4 mol L−1 HCl, quantitative recovery was also obtained. The determination of total selenium was conducted by the application of the
oxidation–reduction process and the analytical procedure for Se (IV). Se (VI) content was calculated as the difference between
total selenium and Se (IV). The detection limit was 0.13 μg L−1. The relative standard deviation was lower than 3.5% for 5 μg L−1 of Se (IV). The trueness of the method was verified by using standardized hydride generation-atomic absorption spectrometry
technique. The results obtained using the EDXRF technique were in good agreement with the ones determined by HG-AAS. The proposed
method was applied to the determination of Se (IV) in surface water and groundwater samples. 相似文献
16.
Based on polyethylene glycol modified single-walled carbon nanotubes, a novel sol–gel fiber coating was prepared and applied
to the headspace microextraction of chlorinated organic carriers (COCs) in textiles by gas chromatography-electron capture
detection. The preparation of polyethylene glycol modified single-walled carbon nanotubes and the sol–gel fiber coating process
was stated and confirmed by infrared spectra, Raman spectroscopy, and scanning electron microscopy. Several parameters affecting
headspace microextraction, including extraction temperature, extraction time, salting-out effect, and desorption time, were
optimized by detecting 11 COCs in simulative sweat samples. Compared with the commercial solid-phase microextraction fibers,
the sol–gel polyethylene glycol modified single-walled carbon nanotubes fiber showed higher extraction efficiency, better
thermal stability, and longer life span. The method detection limits for COCs were in the range from 0.02 to 7.5 ng L−1 (S/N = 3). The linearity of the developed method varied from 0.001 to 50 μg L−1 for all analytes, with coefficients of correlation greater than 0.974. The developed method was successfully applied to the
analysis of trace COCs in textiles, the recoveries of the analytes indicated that the developed method was considerably useful
for the determination of COCs in ecological textile samples. 相似文献
17.
R. K. Singhal H. Basu M. K. T. Bassan M. V. Pimple V. Manisha D. K. Avhad P. K. Sharma A. V. R. Reddy 《Journal of Radioanalytical and Nuclear Chemistry》2012,292(2):675-681
Direct determination of uranium in the concentration range of 8 μg L−1 to mg L−1 in water samples originating from different geochemical environments has been done using Inductively Coupled Plasma-Optical
Emission Spectroscopy (ICP-OES). Uranium detection with 2–3% RSD (relative standard deviation) has been achieved in water
samples by optimizing the plasma power, argon and sheath gas flow. These parameters were optimized for three different emission
lines of uranium at 385.958, 409.014 and 424.167 nm. Interference arising due to the variation in concentration of bicarbonate,
sodium chloride, calcium chloride, Fe and dissolved organic carbon (DOC) on the determination of uranium in water samples
was also cheeked as these are the elements which vary as per the prevailing geochemical environment in groundwater samples.
The concentration of NaHCO3, CaCl2 and NaCl in water was varied in the range 0.5–2.0%; whereas Fe ranged between 1 and 10 μg mL−1 and DOC between 0.1–1%. No marked interference in quantitative determination of uranium was observed due to elevated level
of NaHCO3, CaCl2 and NaCl and Fe and DOC in groundwater samples. Concentration of uranium was also determined by other techniques like adsorptive
striping voltametry (AdSv); laser fluorimetry and alpha spectrometry. Results indicate distinct advantage for uranium determination
by ICP-OES compare to other techniques. 相似文献
18.
Mohana Krishna Reddy Mudiam Rajeev Jain Virendra K. Dua Amit Kumar Singh V. P. Sharma R. C. Murthy 《Analytical and bioanalytical chemistry》2011,401(5):1699-1705
A simple and rapid analytical method based on in-matrix ethyl chloroformate (ECF) derivatization has been developed for the
quantitative determination of bisphenol-A (BPA) in milk and water samples. The samples containing BPA were derivatised with
ECF in the presence of pyridine for 20 s at room temperature, and the non-polar derivative thus formed was extracted using
polydimethylsiloxane solid-phase microextraction (SPME) fibres with thicknesses of 100 μm followed by analysis using gas chromatography–mass
spectrometry. Three alkyl chloroformates (methyl, ethyl and isobutyl chloroformate) were tested for optimum derivatisation
yields, and ECF has been found to be optimum for the derivatisation of BPA. Several parameters such as amount of ECF, pyridine
and reaction time as well as SPME parameters were studied and optimised in the present work. The limit of detection for BPA
in milk and water samples was found to be 0.1 and 0.01 μg L−1, respectively, with a signal-to-noise ratio of 3:1. The limit of quantitation for BPA in milk and water was found to be 0.38
and 0.052 μg L−1, respectively, with a signal-to-noise ratio of 10:1. In conclusion, the method developed was found to be rapid, reliable
and cost-effective in comparison to silylation and highly suitable for the routine analysis of BPA by various food and environmental
laboratories. 相似文献
19.
Dispersive liquid—liquid microextraction coupled with high-performance liquid chromatography—diode-array detection was applied
for the extraction and determination of 11 priority pollutant phenols in wastewater samples. The analytes were extracted from
a 5-mL sample solution using a mixture of carbon disulfide as the extraction solvent and acetone as the dispersive solvent.
After extraction, solvent exchange was carried out by evaporating the solvent and then reconstituting the residue in a mixture
of methanol–water (30:70). The influences of different experimental dispersive liquid—liquid microextraction parameters such
as extraction solvent type, dispersive solvent type, extraction and dispersive solvent volume, salt addition, and pH were
studied. Under optimal conditions, namely pH 2, 165-μL extraction solvent volume, 2.50-mL dispersive solvent volume, and no
salt addition, enrichment factors and limits of detection ranged over 30–373 and 0.01–1.3 μg/L, respectively. The relative
standard deviation for spiked wastewater samples at 10 μg/L of each phenol ranged between 4.3 and 19.3% (n = 5). The relative recovery for wastewater samples at a spiked level of 10 μg/L varied from 65.5 to 108.3%. 相似文献
20.
Zhao RS Yuan JP Li HF Wang X Jiang T Lin JM 《Analytical and bioanalytical chemistry》2007,387(8):2911-2915
Hollow-fiber liquid-phase microextraction (HF-LPME), a relatively new sample preparation technique, has attracted much interest
in the field of environmental analysis. In the current study, a novel method based on hollow-fiber liquid-phase microextraction
with in situ derivatization and gas chromatography–mass spectrometry for the measurement of triclosan in aqueous samples is
described. Hollow-fiber liquid-phase microextraction conditions such as the type of extraction solvent, the stirring rate,
the volume of derivatizing reagent, and the extraction time were investigated. When the conditions had been optimized, the
linear range was found to be 0.05–100 μg l−1 for triclosan, and the limit of detection to be 0.02 μg l−1. Tap water and surface water samples collected from our laboratory and Wohushan reservoir, respectively, were successfully
analyzed using the proposed method. The recoveries from the spiked water samples were 83.6 and 114.1%, respectively; and the
relative standard deviation (RSD) at the 1.0 μg l−1 level was 6.9%. 相似文献