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1.
Chances are examined for the identification and determination of pesticides of different types and polycyclic aromatic hydrocarbons,
46 items, in water and food by means of gas chromatography with time-of-flight mass spectrometry detection. The detection
limits make from 0.01 to 0.5 mg/L if the injected volume of samples is 1 μL; the analytical range is 0.02–10 mg/L. In the
mode of selective ion registration and preliminary preconcentration by liquid and solid-phase extraction, the detection limits
of analytes make from 2 to 100 ng/L in water and from 0.2 to 10 μg/kg for solid samples. 相似文献
2.
Dmitry S. Kosyakov Nikolay V. Ul’yanovskii Sergey A. Pokryshkin Dmitry E. Lakhmanov Oleg A. Shpigun 《International journal of environmental analytical chemistry》2015,95(14):1321-1337
A method for the analytical extraction of mobile species of eightmain transformation products of 1,1-dimethylhydrazine (formaldehyde dimethylhydrazone, acetaldehyde dimethylhydrazone, 2-furaldehyde dimethylhydrazone, 1,1,4,4-tetramethyl-2-tetrazene, N,N-dimethylformamide, N-nitrosodimethylamine, 1-methyl-1H-1,2,4-triazole, and 1-formyl-2,2-dimethylhydrazine) from soils using subcritical acetonitrile at a pressure of 100 bar is proposed. The effects of temperature, number of extraction cycles, and the moisture content of soil samples on the recovery of analytes were studied. It was found that, for soils with high concentrations of lignin humic substances, efficient extraction can be attained with an addition of significant amounts of alkali to the soil (2.5 g/g). Under the optimum conditions, the recovery of analytes was higher than 70% at the extraction time no more than 30 min. A combination of the proposed sample preparation approach with analysis by gas chromatography–tandem mass spectrometry (GC-MS/MS) ensures the determination of the products of unsymmetrical dimethylhydrazine (UDMH) transformation in complex matrixes, such as soils with high concentrations of organic substance with detection limits from 1.8 to 15 µg kg–1 using the direct injection of the extract into the chromatography system. The error of determination at a confidential probability of 0.95 was not worse than 15% even for analyte concentrations close to lower limit of quantitation (LLOQ) values. The method developed is a significant improvement compared to the highly efficient methods previously reported in literature differing from them with simple sample preparation, rapidity, low consumption of reagents, the possibility of simultaneous determination of eight compounds and 1–2 orders of higher sensitivity. It was successfully used for the analysis of real samples of peaty soil from the place of impact of the first step of a carrier rocket. 相似文献
3.
The paper describes a method for the determination of 1-methyl-1H-1,2,4-triazole (MT) in soils contaminated due to space activities at the Baikonur Cosmodrome. MT is the main transformation
product of the primary rocket fuel, 1,1-dimethylhydrazine (UDMH). The analytical procedure is based on gas chromatography
in combination with mass-spectrometric detection. The detection limit of the method was determined to be 0.005 mg kg−1. A series of authentic samples from the fall regions of the burned out first stages of UDMH fueled rockets has been analyzed
disclosing MT concentrations in the range of 0.020 to 100 mg kg−1. 相似文献
4.
Quantification of human and veterinary antibiotics in water and sediment using SPE/LC/MS/MS 总被引:1,自引:0,他引:1
An analytical method was developed and tested for four different groups of veterinary antibiotics in both river water and
sediment matrices. Solid phase extraction (SPE) was used to enrich and to clean up the aqueous sample. Also, Mcllvaine and
ammonium hydroxide buffer solutions were used to extract the compounds from the sediment matrix. High performance liquid chromatography
(HPLC) equipped with tandem mass spectrometry (MS/MS) was used to separate and quantify the samples. The range of recoveries
(in percent) for tetracyclines (TCs), sulfonamides (SAs), macrolides (MLs), and ionophore polyethers (IPs) in the water matrix
were 102.2–124.8, 76.6–124.3, 89.5–114.7, 82.7–117.5 with 1–13 (%) of relative standard deviation respectively with three
different concentrations. For sediment, the percent recovery ranges were 32.8–114.8, 62.4–108.9, 53.4–128.4 and 51.3–105.4
for TCs, SAs, MLs and IPs, respectively. The relative standard deviation ranged from 16 – 27 (%) over three different concentrations.
The limit of quantification (LOQ) was determined by two different methods and calculated to be in the range of 0.01–0.04 μg/l
and 0.3–2.5 μg/kg for TCs, SAs, and MLs in water and sediment, respectively. For IPs, the LOQ was 0.001–0.003 μg/l in river
water and 0.4–3.6 μg/kg for sediment. The sediment concentration measured in an agriculture-influenced river was much higher
than in the overlying water matrix, indicating a high degree of sediment partitioning for these compounds. 相似文献
5.
Mol HG Rooseboom A van Dam R Roding M Arondeus K Sunarto S 《Analytical and bioanalytical chemistry》2007,389(6):1715-1754
The ethyl acetate-based multi-residue method for determination of pesticide residues in produce has been modified for gas
chromatographic (GC) analysis by implementation of dispersive solid-phase extraction (using primary–secondary amine and graphitized
carbon black) and large-volume (20 μL) injection. The same extract, before clean-up and after a change of solvent, was also
analyzed by liquid chromatography with tandem mass spectrometry (LC–MS–MS). All aspects related to sample preparation were
re-assessed with regard to ease and speed of the analysis. The principle of the extraction procedure (solvent, salt) was not
changed, to avoid the possibility invalidating data acquired over past decades. The modifications were made with techniques
currently commonly applied in routine laboratories, GC–MS and LC–MS–MS, in mind. The modified method enables processing (from
homogenization until final extracts for both GC and LC) of 30 samples per eight hours per person. Limits of quantification
(LOQs) of 0.01 mg kg−1 were achieved with both GC–MS (full-scan acquisition, 10 mg matrix equivalent injected) and LC–MS–MS (2 mg injected) for
most of the pesticides. Validation data for 341 pesticides and degradation products are presented. A compilation of analytical
quality-control data for pesticides routinely analyzed by GC–MS (135 compounds) and LC–MS–MS (136 compounds) in over 100 different
matrices, obtained over a period of 15 months, are also presented and discussed. At the 0.05 mg kg−1 level acceptable recoveries were obtained for 93% (GC–MS) and 92% (LC–MS–MS) of pesticide–matrix combinations. 相似文献
6.
R. S. Smirnov I. A. Rodin A. D. Smolenkov O. A. Shpigun 《Journal of Analytical Chemistry》2010,65(12):1266-1272
An approach is proposed for the simultaneous determination of formic acid N,N-dimethylhydrazide and 1-methyl-1-H-1,2,4-triazole (ecotoxicants formed upon the oxidative transformation of unsymmetrical dimethylhydrazine) in soils in the
concentration range 0.05–50 mg/kg using gas chromatography/mass spectrometry. The conditions for the quantitative extraction
of the components by continuous periodic extraction with methanol have been found. The adsorption of formic acid N,N-dimethylhydrazide and 1-methyl-1-H-1,2,4-triazole from solutions by soils of different types has been studied and a method has been proposed for preparing uniform
model soil samples with the required contaminant concentrations. 相似文献
7.
A validated method for simultaneous LCMSMS quantification of nicotine, cocaine, 6-acetylmorphine (6AM), codeine, and metabolites
in 100 mg fetal human brain was developed and validated. After homogenization and solid-phase extraction, analytes were resolved
on a Hydro-RP analytical column with gradient elution. Empirically determined linearity was from 5–5,000 pg/mg for cocaine
and benzoylecgonine (BE), 25–5,000 pg/mg for cotinine, ecgonine methyl ester (EME) and 6AM, 50-5000 pg/mg for trans-3-hydroxycotinine (OH-cotinine) and codeine, and 250–5,000 pg/mg for nicotine. Potential endogenous and exogenous interferences
were resolved. Intra- and inter-assay analytical recoveries were ≥92%, intra- and inter-day and total assay imprecision were
≤14% RSD and extraction efficiencies were ≥67.2% with ≤83% matrix effect. Method applicability was demonstrated with a postmortem
fetal brain containing 40 pg/mg cotinine, 65 pg/mg OH-cotinine, 13 pg/mg cocaine, 34 pg/mg EME, and 525 pg/mg BE. This validated
method is useful for determination of nicotine, opioid, and cocaine biomarkers in brain. 相似文献
8.
Alexander D. Smolenkov Igor A. Rodin Alexey V. Shpak Oleg A. Shpigun 《International journal of environmental analytical chemistry》2013,93(5):351-359
A new decomposition product of 1,1-dimethylhydrazine (UDMH), 1-formyl-2,2-dimethylhydrazine (FDMH), was found in water and soil samples. The formation of FDMH was confirmed by LC-MS and NMR studies. The possibility of FDMH conversion to initial UDMH by alkaline hydrolysis was shown. 相似文献
9.
Sánchez-Rodas D Luis Gómez-Ariza J Oliveira V 《Analytical and bioanalytical chemistry》2006,385(7):1172-1177
A rapid extraction procedure has been developed for speciation of arsenic in chicken tissue. Water, methanol–water (1:1),
and methanol–chloroform (1:1) were tested as extraction media. Individual use of an ultrasonic bath, a microwave oven, or
an ultrasonic probe was not sufficient for quantitative recovery of As(III), dimethylarsinate, monomethylarsonate, As(V),
and arsenobetaine in spiked samples of chicken tissue. A new extraction procedure using a methanol–water mixture and a microwave
oven then an ultrasonic probe enabled extraction of the arsenic species in 7 min with efficiencies ranging from 80 to 100%.
HPLC–UV–HG–AFS was used for the determinations. The extraction procedure was 100% efficient when applied to real samples of
chicken tissue. AsB (48±5 μg As kg −1) and one containing-arsenic feed additive, Nitarsone (227±5 μg As kg −1) were detected. 相似文献
10.
Simultaneous determination of 118 pesticide residues in Chinese teas by gas chromatography-mass spectrometry 总被引:2,自引:0,他引:2
Xin Yang De Chang Xu Jian Wei Qiu Hua Zhang Ying Chun Zhang Ai Jun Dong Ying Ma Jing Wang 《Chemical Papers》2009,63(1):39-46
An efficient and sensitive method for simultaneous determination of 118 pesticide residues in teas has been established and
validated. A multi-residue analysis of pesticides in tea involved extraction with ethyl acetate-hexane, clean-up using gel
permeation chromatography (GPC) and solidphase extraction (SPE), and subsequent identification and quantification of the selected
pesticides by gas chromatography-mass spectrometry (GC-MS). For most of the target analytes, optimized pretreatment processes
led to no significant interference with analysis of sample matrix, and the determination of 118 compounds was achieved in
about 60 min. In the linear range of each pesticide, the correlation coefficient was R
2 ≥ 0.99. At the low, medium and high three fortification levels of 0.05–2.5 mg kg−1, 118 pesticides average recoveries range from 61 % to 121 % and relative standard deviations (RSD) were in the range of 0.6–9.2
% for all analytes. The limits of detection for the method were 0.00030-0.36 mg kg−1, depending on each pesticide. 相似文献
11.
Chen F Chen L Wang Q Zhou J Xue X Zhao J 《Analytical and bioanalytical chemistry》2009,393(3):1073-1079
A rapid and reliable method was developed and applied for the simultaneous determination of 17 organochlorine pesticides (OCPs)
in propolis. After extraction with hexane and acetone (1:1, v/v), four sorbents (florisil, silica, graphitized carbon, and
tandem graphitized carbon plus florisil) were assayed for the clean-up step. The elution solvents hexane and ethyl acetate
(1:1, v/v), hexane and dichloromethane (3:7, v/v), and ethyl acetate and hexane (2:8, v/v) were studied. The results showed
that the combination of the tandem graphitized carbon and florisil cartridge with the elution solvent of 6mL of ethyl acetate
and hexane (2:8, v/v), which was capable of eliminating matrix interference and providing colorless eluates, was the most
efficient clean-up procedure for propolis extracts when testing for OCPs. The analytical technique employed was gas chromatography
with electron capture detection (GC–ECD). The correlation coefficients from linear regression for the analyzed concentrations
(5∼100 μg/kg) were >0.9961. The limits of detection (LODs) varied between 0.8 μg/kg for 4,4′-DDE and 11.4 μg/kg for endosulfan
II, and the limits of quantitation (LOQs) ranged from 2.6 to 38.1 μg/kg. The average recoveries varied between 62.6 and 109.6%.
Relative standard deviations (RSD%) ranged from 0.8 to 9.4%. Sample analysis indicated that 4,4′-DDE was detected more often
in propolis than other pesticides, such as β-HCH, δ-HCH and heptachlor.
Figure GC-ECD chromatogram of a standard solution with 0.1 mg/L of OCPs 相似文献
12.
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
13.
Aguilera-Luiz MM Plaza-Bolaños P Romero-González R Vidal JL Frenich AG 《Analytical and bioanalytical chemistry》2011,399(8):2863-2875
A rapid multi-analyte method has been developed for the simultaneous determination of pesticides and mycotoxins in milk by
ultra high-performance liquid chromatography coupled to triple quadrupole mass spectrometry (UHPLC–QqQ–MS/MS). A variety of
methodologies has been evaluated, including solid-phase extraction (SPE), “dilute-and-shoot” (liquid–liquid extraction-based
procedures), and QuEChERS (quick, easy, cheap, effective, rugged, and safe)-based methods. The optimization and development
process was carried out considering that the maximum residue level for aflatoxin M1 (AFM1) in milk in the European Union (EU)
is set at 0.05 μg kg−1, which is the lowest tolerance in the target compounds. The selected method consisted of an extraction by SPE using C18 as
sorbent and methanol as elution solvent. The final determination was performed by UHPLC–QqQ–MS/MS. Matrix-matched standard
calibration was used for quantification, obtaining recoveries in the range 60–120% with relative standard deviations <25%,
at three spiking levels: 0.5, 10, and 50 μg kg−1 (ten times lower for AFM1). Limits of quantification ranged from 0.20 to 0.67 μg kg−1, which were always below or equal to the established tolerance levels by the EU. Finally, the selected method was applied
to different types of milk. 相似文献
14.
Determination of Abamectin Residues in Avocados by Microwave-Assisted Extraction and HPLC with Fluorescence Detection 总被引:1,自引:0,他引:1
Javier Hernández Borges Lidia M. Ravelo-Pérez Estrella M. Hernández-Suárez Aurelio Carnero Miguel Ángel Rodríguez-Delgado 《Chromatographia》2008,67(1-2):69-75
In this article a new analytical method for the confirmation and quantification of abamectin residues in avocados is described.
The method allows a fast analysis of abamectin homologues using microwave assisted extraction (MAE), solid-phase extraction
(SPE) and high-performance liquid chromatography (HPLC) with fluorescence (FL) detection using trifluoroacetic anhydride (TFAA)
and N-methylimidazole (NMIM) as derivatizing agents. The mobile phase consisted of water, methanol and acetonitrile (5:47.5:47.5
v/v/v) and was pumped at a rate of 1.1 mL min−1 (isocratic elution). Homogenized avocado samples were extracted once with 20 mL acetonitrile:water 4:1 (v/v) in a microwave oven for 26 min at 700 W with a maximum temperature of 80 °C. MAE operational parameters were optimized by
means of an experimental design. Extracts were cleaned using C18 SPE cartridges. Average recoveries of the method at four spiked levels (0.005, 0.01, 0.10 and 1.0 mg kg−1) were found to be in the range 90–100% with good precision (RSD < 12%). The limits of detection (LODs) and quantification
(LOQs) of the whole method were 0.001 and 0.003 mg kg−1, respectively, which are lower than the maximum residue limit (MRL) established by the Spanish and the European legislation
in avocados (0.01 mg kg−1). Several avocado samples previously treated with the pesticide were also analyzed. 相似文献
15.
Haiyang Jiang Shuangyang Ding Fei Xu Sijun Zhao Jihong He Jinfeng Liu Xiaolin Hou Jianzhong Shen 《Chromatographia》2007,66(5-6):411-414
Eprinomectin is a novel and potent antiparasitic animal health drug. An analytical procedure for the determination of EPR
in bovine urine and feces has been developed. The urine sample was centrifuged and alkalized with ammonia following solid
phase extraction. The fecal sample was extracted with acetonitrile, defatted with hexane, cleaned-up using C18 cartridge.
All samples were analyzed by high performance liquid chromatography with fluorescence detection after derivatization with
N-methylimidazole. The limits of detection are 0.5 ng mL−1 and 0.5 ng g−1, respectively. Fortified at 2, 10, 50, and 100 ng mL−1(ng g−1), inter-assay recoveries of EPR in cattle urine and feces were in the range of 87.9–91.5% and 78.6–86.3%, with coefficients
of variation of 5.4–10.2% and 1.4–7.2%, respectively. Intra-assay mean recoveries of the analytes were 82.2–86.5% and 79.6–87.3%,
with coefficients of variation of 7.8–11.5% and 6.3–7.8%, respectively. The method was used to study the excretion of eprinomectin
in bovine urine and feces after subcutaneous administration at a dose of 0.5 mg kg−1. 相似文献
16.
P. Parrilla P. Kaim E. A. Hogendoorn R. A. Baumann 《Fresenius' Journal of Analytical Chemistry》1999,363(1):77-82
In the development of a screening method for the determination of residues of mecoprop in soils involving coupled-column RPLC-UV
(228 nm) the cleanup performance of a 5 μm GFF-II internal surface reversed phase (ISRP, Pinkerton) analytical column (50
× 4.6 mm I.D.) as a first column was investigated. In comparison to an analytical C18 column the ISRP column substantially
improved the separation between acidic analyte and co-extracted humic substances. Under the selected coupled-column conditions
soil extracts obtained after hydrolysis with an aqueous alkaline solution, acidifying and centrifugation could be analyzed
directly allowing the determination of mecoprop in soils to a level of about 0.02 mg/kg. A rapid concentration step on a 100
mg C18 solid phase extraction (SPE) cartridge was adopted into the procedure providing a limit of detection (S/N = 3) of 0.01
mg/kg of mecoprop in soil. The method was validated by analyzing freshly spiked soil samples and samples with aged residues.
In case of freshly spiked samples the overall recovery was 87% (n = 18, spiked level 0.02–8.0 mg/kg) with a repeatability
of 6.8% and a reproducibility of 8.3%. No significant decrease of the recovery was observed for samples with aged residues
(n = 15, spiked level 0.1 and 8.0 mg/kg) during a storage of 29 days in the refrigerator at about 4 °C; a storage of 67 days
provided a mean recovery of 76% (n = 14, spiked level 8.0 mg/kg).
Received: 4 May 1998 / Revised: 11 July 1998 / Accepted: 18 July 1998 相似文献
17.
Mohammad Wasim Nasir Khalid Azeem Asif Mohammad Arif Jamshed Hussain Zaidi 《Journal of Radioanalytical and Nuclear Chemistry》2012,292(3):1153-1159
Mineral contents of strawberry, collected from different farms of Islamabad were analysed by semi-absolute k
0-instrumental neutron activation analysis and atomic absorption spectrophotometry. The samples were irradiated at two research
reactors located in Pakistan Institute of Nuclear Science & Technology (PINSTECH), Islamabad. The analytical methodologies
were validated by analysing reference materials, IAEA-336 (lichen) and IAEA-V-10 (hay powder). In all the samples, a total
of 26 elements were quantified, among them 16 elements (Ca, Cd, Cl, Co, Cr, Cs, Fe, K, Mg, Mn, Na, Pb, Ru, Sc, Sr and Zn)
were found in all the samples. The determined elemental concentrations in strawberry were compared with the reported values
from other countries. In comparison with the mineral contents of other fruits, strawberry stands best source of Mn and the
second most important source of K after banana. Intake of trace metals through this source was calculated and it was found
that strawberry provides Mn (1.95–3.68 mg/kg), Cr (19.2–46.3 × 10−3 mg/kg), Fe (3.45–8.72 mg/kg), K (1,520–1,670 mg/kg) and Mg (100–220 mg/kg), which forms 26, 19, 14, 7 and 7% of the recommended
dietary allowances for the respective metals. The daily intake of Cd and Pb were compared with the provisional tolerable weekly
intake defined by FAO/WHO. 相似文献
18.
Christina Schiborr Gunter P. Eckert Gerald Rimbach Jan Frank 《Analytical and bioanalytical chemistry》2010,397(5):1917-1925
Curcumin, a lipophilic polyphenol derived from the rhizome of the plant turmeric (Curcuma longa), might be useful in the prevention and treatment of a number of degenerative brain disorders, including glioma multiforma
and Alzheimer’s disease. Thus, there is growing interest in measuring curcumin concentrations in the brain and other target
tissues in relevant animal models. We therefore developed and validated (according to the Food and Drug Administration guidelines
for bioanalytical method validation), a simple, fast and reliable method for the quantification of curcumin in biological
matrices by fast high-performance liquid chromatography with fluorescence detection. This method involves a simple extraction
with 95% ethyl acetate and 5% methanol, rapid separation (<2 min if external standards and <4 min if the internal standard
β-estradiol 17-acetate is used) on a Jasco Reprosil-Pur Basic C18 column (75 × 2 mm, 1.8 μm) with an eluent of acetonitrile, methanol, de-ionised water and acetic acid (49:20:30:1, v/v; flow rate, 0.4 mL/min) and fluorescence detection (excitation wavelength, 420 nm; emission wavelength, 470 nm). The method
is selective, precise (<15% RSD at the lower limit of quantification), accurate (<15% of the coefficient of variation at the
lower limit of quantification) and sensitive over a linear range of 0.05–10 μg/mL for curcumin. The developed method was used
for the quantification of curcumin in the brains of mice force-fed (50 mg/kg bw) or i.p. injected (100 mg/kg bw) with curcumin.
Brain curcumin concentrations of the mice were below the limit of detection at 30, 60 and 120 min after oral gavage and reached
4–5 μg/g brain 20–40 min after i.p. injection. In conclusion, the developed and validated method should be useful for the
accurate and precise quantification of curcumin in target organs from relevant animal models of human diseases. 相似文献
19.
M. Vahl Anette Graven René K. Juhler 《Fresenius' Journal of Analytical Chemistry》1998,361(8):817-820
A fast, sensitive and specific method for routine determination of residues from Chlormequat (CAS no. 7003-89-6) is described.
The method is based on a simple clean-up using an SPE-C18 cartridge, high-performance liquid chromatography on a standard C18 column (Spherisorb S5 ODS1) and specific detection and quantification by electrospray mass spectrometry (LC-MS/MS). 13C-Chlormequat was synthesised for use as internal standard. Samples were extracted with methanol – water – acetic acid. Internal
standard and ammonium acetate were added before C18-cartridge clean up and residues eluted with methanol – water – acetic acid, containing 50 mM ammonium acetate. Chromatographic
separation was achieved using a solvent composed of acetonitrile – methanol – water – acetic acid (53:21:25:1 by volume),
containing 50 mM ammonium acetate. Electrospray ionisation mass spectrometry was employed using m/z 58 (daughter ion of the
Chlormequat quaternary ammonium ion, m/z 122) and m/z 61 (daughter ion of the 13C-Chlormequat quaternary ammonium ion, m/z 125) for quantification. The LC analysis time was 15 min and the limit of detection
of the analytical method was 9 μg/kg. The performance of the method was demonstrated analysing grain material from an inter-comparison
study. In Denmark the primary use of Chlormequat chloride (CCC, cycocel, or chlorocholin chloride, CAS no. 999-81-5) is for
winter cereals and 11 such winter wheat samples from the Danish National Pesticide Survey were analysed. Residue contents
were from below 0.01 up to 0.45 mg/kg, and thus below the EU maximum residue level of 2.0 mg/kg for wheat.
Received: 22 December 1997 / Revised: 29 January 1998 / Accepted: 31 January 1998 相似文献
20.
Russo MV Notardonato I Cinelli G Avino P 《Analytical and bioanalytical chemistry》2012,402(3):1373-1381
A solid-phase extraction (SPE) method was developed for extraction and analysis of six phthalate esters in wine samples using
Carbograph 1 sorbent. The SPE procedure allowed efficient recovery of the investigated phthalates ranging between 78% and
105% with a relative standard deviation (RSD) ≤6.5 for an ethanolic phthalic acid ester (PAE) standard solution and between
73–71% and 96–99% with a RSD ≤8.4 for red wine samples spiked with 20 and 50 ng mL−1 of PAE, respectively. The adsorption isotherms and breakthrough curves for Carbograph 1/water solution were reported. Gas
chromatography coupled with an ion-trap mass spectrometer detector (GC/IT-MS) was used for analysis. The instrumental analytical
protocol was found to yield a linear calibration in the range 0.01-10.0 μg mL−1 with R
2 values ≥0.9992. The limits of detection in GC/IT-MS (SIM mode) vary between 0.2 and 14 ng mL−1 (RSD ≤5.6) whereas the limits of quantification range between 0.5 and 25 ng mL−1 (RSD ≤5.9); the intra- and inter-day repeatabilities calculated as RSD for wine samples, were between 0.9–7.8 and 1.0–10.5,
respectively. The analytical method developed was applied to several commercial wine samples. Furthermore, the investigated
methods are simple, reliable, reproducible, and not expensive. 相似文献