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1.
José Luis Martínez Vidal Antonia Garrido Frenich María de las Nieves Barco Bonilla Roberto Romero-González Juan Antonio Padilla Sánchez 《Analytical and bioanalytical chemistry》2009,395(5):1551-1562
A simple and rapid method based on pressurized liquid extraction has been validated for the simultaneous extraction of polychlorinated
biphenyls (PCBs) and polycyclic aromatic hydrocarbons (PAHs) from agricultural soil samples. Effective extraction was carried
out in less than 17 min for all the studied compounds, and good recoveries were obtained for PAHs and PCBs, ranging from 70%
to 112%, when blank samples were spiked at 2.5 μg kg−1, except for naphthalene with recoveries close to 40%. The separation and determination were performed by gas chromatography
coupled to tandem mass spectrometry using a triple quadrupole mass analyzer. The target compounds were detected by electron
impact with selected reaction monitoring, and mass spectrometric conditions were optimized in order to increase selectivity
and sensitivity. The developed method was validated, and matrix-matched calibration was used for quantification purposes.
Repeatability and interday precision ranged from 0.9% to 16.8% and from 1.6% to 22.3%, respectively. Limits of quantification
ranged from 0.07 to 2.50 μg kg−1. The proposed method was applied to the analysis of agricultural soil samples collected from Almeria (Spain), and PAHs and
PCBs were detected in some samples at concentrations ranging from 0.1 to 210 μg kg−1. 相似文献
2.
Determination of tetracycline residues in soil by pressurized liquid extraction and liquid chromatography tandem mass spectrometry 总被引:2,自引:0,他引:2
Vicente Andreu Pablo Vazquez-Roig Cristina Blasco Yolanda Picó 《Analytical and bioanalytical chemistry》2009,394(5):1329-1339
An optimized extraction and cleanup method for the analysis of chlortetracycline (CTC), doxycycline (DC), oxytetracycline
(OTC) and tetracycline (TC) in soil is presented. Soil extraction in a pressurized liquid extraction system, followed by extract
clean up using solid-phase extraction (SPE) and tetracycline determination by liquid chromatography tandem mass spectrometry
(LC-MS/MS) provided appropriate efficiency and reproducibility. Different dispersing agents and solvents for soil extraction
and several SPE cartridges for cleanup were compared. The best extraction results were obtained using ethylenediamine tetraacetic
acid-treated sand as dispersing agent, and water at 70 °C. The most effective cleanup was obtained using Strata-XTM sorbent in combination with a strong anion exchange cartridge. Recoveries ranged from 71% to 96% and precision, as indicated
by the relative standard deviations, was within the range of 8–15%. The limits of quantification (LOQs) by using LC-MS/MS,
based on signal-to-noise ratio (S/N) of 10, ranged from 1 μg kg−1 for TC to 5 μg kg−1 for CTC. These results pointed out that this technique is appropriate to determine tetracyclines in soils. Analysis of 100
samples taken in the Valencian Community revealed that, in soil, up to 5 μg kg−1 CTC, 15 μg kg−1 OTC, 18 μg kg−1 TC, and 12 μg kg−1 DC could be detected. Detection of the analytes in several samples, which typify great part of the Spanish agricultural soils,
should be outlined as most important result of this study.
Electronic supplementary material The online version of this article (doi: ) contains supplementary material, which is available to authorized users. 相似文献
3.
Certified reference material for quantification of polycyclic aromatic hydrocarbons in sediment from the National Metrology Institute of Japan 总被引:2,自引:0,他引:2
Nobuyasu Itoh Yoshie Aoyagi Akiko Takatsu Takashi Yarita 《Analytical and bioanalytical chemistry》2009,393(8):2039-2049
The National Metrology Institute of Japan has issued a certified reference material (CRM) of freshwater lake sediment for
polycyclic aromatic hydrocarbon (PAHs) analyses. The certification used three extraction techniques: pressurized liquid extraction
(PLE) with toluene, PLE with dichloromethane/ethyl acetate (1:1 by volume), and alkaline extraction (1 M KOH in methanol)
in combination with microwave-assisted extraction. Both gas chromatography/mass spectrometry (GC/MS) and liquid chromatography/dopant-assisted
atmospheric pressure photoionization/MS (LC/DA-APPI/MS) analyses were used. Certified values are provided for 18 PAHs at 1–25 μg
kg−1 except for perylene (2.08 × 103 μg kg−1), and information values are provided for two. Since the values of PAHs in the CRM are much lower than those in other CRMs
and are comparable to those found at sites with little human influence, the CRM is suitable for PAH monitoring in sediment
and soil samples. 相似文献
4.
Quintana JB Rodil R López-Mahía P Muniategui-Lorenzo S Prada-Rodríguez D 《Analytical and bioanalytical chemistry》2007,388(5-6):1283-1293
A selective analytical method for the determination of nine organophosphate triesters and triphenylphosphine oxide (TPPO)
in outdoor particulate matter is presented. It involves a fully automated pressurised liquid extraction (PLE) step, integrating
an alumina clean-up process, and subsequent determination by large-volume injection gas chromatography–positive chemical ionisation–tandem
mass spectrometry (LVI-GC–PCI–MS/MS). The extraction variables (solvent, amount of adsorbent, temperature, time and number
of cycles) were optimised using a multicriteria strategy which implements a desirability function that maximises both extraction
and clean-up efficiencies while searching for the best-compromise PLE conditions. The final method affords quantification
limits of between 0.01 and 0.3 μg g−1 and recoveries of >80%, with the exceptions of the most polar analytes, TCEP and TPPO (~65%) for both urban dust and PM10
samples. Moreover, the method permitted the levels of these compounds in dust deposited outdoors (between LOD and 0.5 μg g−1 for TEHP) and PM10 samples (between LOD and 2.4 μg m−3 for TiBP) to be measured and reported for the first time.
Electronic supplementary material The online version of this article (doi:) contains supplementary material, which is available to authorized users. 相似文献
5.
Fumonisins B1 (FB1) and fumonisin B2 (FB2) are the main members of a family of mycotoxins produced by Fusarium verticillioides, Fusarium proliferatum, and other fungi species of the section Liseola. The present work shows the results of comparative studies using two different procedures for the analysis of fumonisins
in maize and maize-based samples. The studied analytical methods involve extraction with methanol/water, dilution with PBS,
and clean-up through immunoaffinity columns. Two reagents (o-phthaldialdehyde and naphthalene-2,3-dicarboxaldehyde) were studied for formation of fluorescent derivatives. The separation
and identification were carried out by high-performance liquid chromatography with fluorescence detection. The optimized method
for analysis of fumonisins in maize involved extraction with methanol/water (80:20), clean-up with an immunoaffinity column,
and derivatization with naphthalene-2,3-dicarboxaldehyde (NDA). The limit of detection was 20 μg kg−1 for FB1 and 15 μg kg−1 for FB2. Recoveries of FB1 and FB2 ranged from 79% to 99.6% for maize fortified at 150 μg kg−1 and 200 μg kg−1, respectively, with within-day RSDs of 3.0 and 2.7%. The proposed method was applied to 31 samples, and the presence of fumonisins
was found in 14 samples at concentrations ranging from 113 to 2,026 μg kg−1. The estimated daily intake of fumonisins was 0.14 μg kg−1 body weight per day. 相似文献
6.
Lina Kantiani Marinella Farré Josep Manuel Grases i Freixiedas Damià Barceló 《Analytical and bioanalytical chemistry》2010,398(3):1195-1205
A fully automated method has been developed for analysis of eighteen antibacterial compounds, including penicillins, cephalosporins
and sulfonamides, in animal feed with limits of quantification in the range 0.25–5.79 μg kg−1. The method is based on pressurized liquid extraction of 3 g homogenized feed with water and online clean-up of 500 μL of
the extract with C18HD cartridges. The purified sample was directly analysed by liquid chromatography–electrospray tandem mass spectrometry (SPE–LC–ESI-MS–MS).
Chromatographic separation was achieved within 10 min by use of a C12 Phenomenex Hydro-RP reversed-phase analytical column and a mobile phase gradient (water + 0.1% formic acid–methanol + 0.1%
formic acid). The method was validated, revealing capability for detection of concentrations as low as 0.09 μg kg−1, decision limits (CCα) and detection capabilities (CCβ) in the range 10–174 μg kg−1 and 22–182 μg kg−1, respectively, and inter-day precision ranging from 0.7 to 8.3%. Recovery, with internal standard correction, was in the
range 93–134% for all analytes. The method was then applied to analysis of fifteen feed samples, nine of which contained at
least one antimicrobial at concentrations between 0.006 and 1.526 mg kg−1. The performance data and results from the method were compared with those from a previous method developed by our group,
using offline SPE, by analyzing the same set of samples by both methods. The online SPE approach resulted in slightly improved
sensitivity, with LODs of 0.09–2.12 μg kg−1 compared with 0.12–3.94 μg kg−1 by the offline approach. In general, better recovery was achieved by use of online purification (for 72% of the analytes)
and the correlation between the two methods was good. The main advantages of the new online method are rapid and automated
sample pre-treatment, and reduction of sample manipulation, enabling high-throughput analysis and highly accurate results.
Because of all these characteristics, the proposed method is applicable and could be deemed necessary within the field of
food control and safety. 相似文献
7.
Clémens S Monperrus M Donard OF Amouroux D Guérin T 《Analytical and bioanalytical chemistry》2011,401(9):2699-2711
Methylmercury (MeHg) and total mercury (THg) in seafood were determined using species-specific isotope dilution analysis and
gas chromatography combined with inductively coupled plasma mass spectrometry. Sample preparation methods (extraction and
derivation step) were evaluated on certified reference materials using isotopically enriched Hg species. Solid–liquid extraction,
derivation by propylation and automated agitation gave excellent accuracy and precision results. Satisfactory figures of merit
for the selected method were obtained in terms of limit of quantification (1.2 μg Hg kg−1 for MeHg and 1.4 μg Hg kg−1 for THg), repeatability (1.3–1.7%), intermediate precision reproducibility (1.5% for MeHg and 2.2% for THg) and trueness
(bias error less than 7%). By means of a recent strategy based on accuracy profiles (β-expectation tolerance intervals), the
selected method was successfully validated in the range of approximately 0.15–5.1 mg kg−1 for MeHg and 0.27–5.2 mg kg−1 for THg. Probability β was set to 95% and the acceptability limits to ±15%. The method was then applied to 62 seafood samples
representative of consumption in the French population. The MeHg concentrations were generally low (1.9–588 μg kg−1), and the percentage of MeHg varied from 28% to 98% in shellfish and from 84% to 97% in fish. For all real samples tested,
methylation and demethylation reactions were not significant, except in one oyster sample. The method presented here could
be used for monitoring food contamination by MeHg and inorganic Hg in the future to more accurately assess human exposure. 相似文献
8.
Ghanem A Bados P Perreau F Benabdallah R Plagellat C de Alencastro LF Einhorn J 《Analytical and bioanalytical chemistry》2008,391(1):345-352
A multiresidue method has been developed to analyze atrazine (ATZ), diuron (DIU), and their major degradation products, desethylatrazine
(DEA), desisopropylatrazine (DIA), and dichlorophenylmethylurea in sewage sludge. Liquid chromatography coupled to electrospray
tandem mass spectrometry (LC–ESI-MS–MS) allowed, in the multiple-reaction monitoring mode, the simultaneous analysis of these
pesticides in only one run after their extraction with ethyl acetate–dichloromethane 90:10 (v/v) and a cleanup on a Florisil column. Stable isotopically labeled ATZ and DIU were used as internal standards to overcome
matrix effects during the pesticide quantification. Using fortified samples, the method gave rise to 86–115% as mean recovery
values depending on the analyte. Limits of detection (LODs) and of quantification (LOQs) ranging from 0.3 (DIA) to 1.5 (DEA)
μg kg−1 dw and from 0.4 (DIA) to 2.0 (DEA) μg kg−1 dw, respectively, were sufficient to achieve the monitoring of these molecules in sludge from wastewater treatment plants
of the Ile-de-France region. 相似文献
9.
Simultaneous determination of six major ergot alkaloids and their epimers in cereals and foodstuffs by LC–MS–MS 总被引:1,自引:0,他引:1
This paper describes a new and rapid method for accurate quantification of the six ergot alkaloids, ergometrine, ergotamine,
ergosine, ergocristine, ergocryptine, and ergocornine, by liquid chromatography–tandem mass spectrometry (LC–MS–MS). The six
ergot alkaloids studied have been defined by the European Food Safety Authority (EFSA) as among the most common and physiologically
active ones. In addition, the method enables the quantification of the corresponding six epimers (ergo-inines) of these ergot alkaloids. This is of considerable importance in terms of the differences in toxicity of the isomeric forms.
The method involves extraction under alkaline conditions using a mixture of acetonitrile and ammonium carbonate buffer followed
by a rapid clean-up using dispersive solid-phase extraction with PSA (primary secondary amine) and a short chromatographic
LC-run (21 min) with subsequent MS–MS detection. The method was developed and validated using ten different cereal and food
samples. The major strength of the new method compared with previously published techniques is the simplicity of the clean-up
procedure and the short analysis time. The limits of quantification were 0.17 to 2.78 μg kg−1 depending on the analyte and matrix. Recovery values for the 12 ergot alkaloids spiked into ten different matrices at levels
of 5, 50, and 100 μg kg−1 were between 69 and 105% for 85 of 90 recovery measurements made over six days. Measurement uncertainty values were highly
satisfactory. At a concentration level of 5 μg kg−1 the expanded measurement uncertainty ranged from ±0.56 to ±1.49 μg kg−1, at a concentration level of 100 μg kg−1 the expanded measurement uncertainty ranged from ±8.9 to ±20 μg kg−1. Both LOQs and measurement uncertainties were dependent on the analyte but almost independent of the matrix. The method performance
was satisfactory when tested in a mini-intercomparison study between three laboratories from three different countries.
Electronic supplementary material The online version of this article (doi:) contains supplementary material, which is available to authorized users. 相似文献
10.
A confirmatory and quantitative method based on liquid chromatography–electrospray ionization tandem mass spectrometry (LC-ESI/MS/MS)
has been developed for simultaneous determination of seven photoinitiator residues: benzophenone, (1-hydroxycyclohexyl)phenylketone
(Irgacure 184), isopropylthioxanthone (ITX), 2-ethylhexyl-(4-dimethylamino)benzoate (EHA or EHDAB), 2-methyl-1-[4-(methylthio)phenyl]-2-(4-morpholinyl)-1-propanone
(Irgacure 907), (2,4,6-trimethylbenzoyl)diphenylphosphine oxide (TPO) and 2-benzyl-2-(dimethylamino)-1-(4-morpholinophenyl)-1-butanone
(Irgacure 369) in packaged milk and related packaging materials. Residues of photoinitiators were extracted from milk using
acetonitrile, and further enriched and purified on HLB solid-phase extraction cartridges prior to being analyzed by LC-ESI/MS/MS
with selected reaction monitoring mode, while photoinitiators in packaging materials were extracted using the same solvent.
Satisfactory recovery (from 80 to 111%), intra- and inter-day precision (below 12%), and low limits of quantification (from
0.1 to 5.0 μg kg−1) were evaluated from spiked samples at three concentration levels (5.0, 10.0 and 25.0 μg kg−1 for Irgacure 184 and 2.5, 5.0 and 25.0 μg kg−1 for others). These excellent validation data suggested the possibility of using the LC-ESI/MS/MS method for simultaneous
determination of low-level photoinitiator residues migrating from printed food-packaging materials into milk. The method has
been successfully applied to the analysis of real samples of different fat contents ranging from 8 to 30 g L−1. The photoinitiator residues were revealed to be higher in milk with higher fat content and the most important contaminations
were benzophenone and ITX in concentration ranges of 2.84–18.35 and 0.83–8.87 μg kg−1, respectively. 相似文献
11.
A multi-component method focussing on thorough sample preparation has been developed for simultaneous analysis of swine manure
for three classes of antibiotic—tetracyclines, sulfonamides, and tylosin. Liquid manure was initially freeze-dried and homogenised
by pulverization before extraction by pressurised liquid extraction. The extraction was performed at 75°C and 2,500 psig in
three steps using two cycles with 0.2 mol L−1 citric acid buffer (pH 4.7) and one cycle with a mixture of 80% methanol with 0.2 mol L−1 citric acid (pH 3). After liquid–liquid extraction with heptane to remove lipids, the pH of the manure was adjusted to 3
with formic acid and the sample was vacuum-filtered through 0.6 μm glass-fibre filters. Finally the samples were pre-concentrated
by tandem SPE (SAX-HLB). Recoveries were determined for manure samples spiked at three concentrations (50–5,000 μg kg−1 dry matter); quantification was achieved by matrix-matched calibration. Recoveries were >70% except for oxytetracycline (42–54%),
sulfadiazine (59–73%), and tylosin (9–35%) and did not vary with concentration or from day-to-day. Limits of quantification
(LOQ) for all compounds, determined as a signal-to-noise ratio of 10, were in the range 10–100 μg kg−1 dry matter. The suitability of the method was assessed by analysis of swine manure samples from six different pig-production
sites, e.g. finishing pigs, sows, or mixed production. Residues of antibiotics were detected in all samples. The largest amounts
were found for tetracyclines (up to 30 mg kg−1 dry matter for the sum of CTC and ECTC). Sulfonamides were detected at concentrations up to 2 mg kg−1 dry matter (SDZ); tylosin was not detected in any samples.
相似文献
12.
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
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.
The worldwide contamination of winery by-products by mycotoxins may present a serious hazard to human and animal health. Mycotoxins
are secondary metabolites of fungi with possible adverse effects on humans, animals, and crops that result in illnesses and
economic losses. Mycotoxins are under continuous survey in Europe, but the regulatory aspects still need to be set up for
winery by-products, which may be used in animal feed. The aim of this study was to implement a simple but reliable analytical
methodology for ochratoxin A (OTA) quantification in grape pomaces in order to perform a survey of samples from the Douro
Demarcated Region, Portugal. The method involved a unique preparation step, solvent extraction, followed by high-performance
liquid chromatography (HPLC) with fluorescence (FL) detection. A comparative study was performed with two extraction solvents
(ethyl acetate and methanol) as well as using extraction on an immunoaffinity column. The linearity range for OTA analysis
was 0.05–23.5 μg L−1 with a detection limit of 0.05 μg L−1 and a precision (expressed by the coefficient of variation under repeatability conditions) of 0.4–14.7%. The percentage of
recovery was on average 23.5 ± 3.6% (extraction with ethyl acetate) or 70.1 ± 2.5% (extraction with 70% methanol). Accounting
for the recovery factor and the chromatographic detection limit, as well as the preconcentration factor, the limit of detection
in grape pomaces is 0.04 μg kg−1 (ethyl acetate extraction) and 0.33 μg kg−1 (methanol extraction). Samples from 12 out of 13 sites in the Douro Demarcated Region showed OTA presence with concentrations
not exceeding 0.4 μg kg−1. Both developed methods for evaluation of OTA in grape pomace are simple but efficient.
Figure Extraction of ochratoxin A (OTA) from grape pomaces allows simple but efficient quantification of OTA in winery by-products
by HPLC-FL 相似文献
15.
This paper reports a novel approach for the detection, confirmation, and quantification of 15 selected pyrethroid pesticides,
including pyrethins, and two metabolites of dithiocarbamates in foods by ultra-performance liquid chromatography–tandem mass
spectrometry (UPLC–MS–MS). The proposed method makes use of a modified QuEChERS (quick, easy, cheap, effective, rugged, and
safe) procedure that combines isolation of the pesticides and sample cleanup in a single step. Analysis of pyrethroids and
dithiocarbamate metabolites was performed by UPLC–MS–MS operated with electrospray and atmospheric pressure chemical ionization,
respectively. Two specific precursor–product ion transitions were acquired per target compound in multiple reaction monitoring
(MRM) mode. Such acquisition achieved the minimum number of identification points according to European Commission (EC) document
no. SANCO/10684/2009, thus fulfilling the EC point system requirement for identification of contaminants in samples. The method
was validated with a variety of food samples. Calibration curves were linear and covered from 1 to 800 μg kg−1 in the sample for all target compounds. Average recoveries, measured at mass fractions of 10 and 100 μg kg−1 for pyrethroids and 5 and 50 μg kg−1 for dithiocarbamate metabolites, were in the range of 70–120% for all target compounds with relative standard deviations
below 20%. Method limits of quantification (MLOQ) were 10 μg kg−1 and 5 μg kg−1 for pyrethroids and dithiocarbamate metabolites, respectively. The method has been successfully applied to the analysis of
600 food samples in the course of the first Hong Kong total diet study with pyrethroids and metabolites of dithiocarbamates
being the pesticides determined. 相似文献
16.
A pressurized liquid extraction (PLE) method has been optimized for the determination of polycyclic aromatic hydrocarbons (PAHs) in soil samples and it was compared with ultrasonic extraction. The extraction step was followed by gas chromatography-triple quadrupole mass spectrometry (GC-QqQ-MS/MS) analysis. Parameters such as type of solvent, extraction time, extraction temperature and number of extractions were optimized. There were no significant differences among the two extraction methods although better extraction efficiencies were obtained when PLE was used, minimizing extraction time and solvent consumption. PLE procedure was validated, obtaining limits of detection (LODs) ranging from 0.02 to 0.75 μg kg−1 and limits of quantification (LOQs) ranging from 0.07 to 2.50 μg kg−1 for the selected PAHs. Recoveries were in the range of 59-110%, except for naphthalene, which was the most volatile PAH. Finally, the method was applied to real soil samples from Southeast of Spain. PAHs concentrations were low, and phenanthrene, pyrene, fluorene, benzo[a]pyrene and chrysene were the most frequently detected analytes in the samples. 相似文献
17.
L. Giannetti F. Longo F. Buiarelli M. V. Russo B. Neri 《Analytical and bioanalytical chemistry》2010,398(2):1017-1023
A specific, sensitive and robust liquid chromatography tandem mass spectrometry method for determining oxytetracycline, tetracycline,
chlortetracycline and doxycycline in royal jelly and honey samples is presented. Extraction of drug residues was performed
by ammonium acetate buffer as extractant followed by a clean-up with metal chelate affinity chromatography and solid-phase
extraction. Tetracycline analysis was performed using liquid chromatography–electrospray ionisation–tandem mass spectrometry.
The presented method is the first validated for royal jelly and in accordance with the requirements set by Commission Decision
2002/657/EC. Recoveries of the methods, calculated spiking the samples at 5.0, 10.0, 20.0 and 30.0 μg kg−1, were 79% to 90% for honey and 77% to 90% for royal jelly. The intra-day precision (RSD) ranged between 8.1% and 15.0% for
honey and from 9.1% to 16.3% for royal jelly, while inter-day precision values were from 10.2% to 17.6% and from 10.6% to
18.4% respectively for honey and royal jelly. Linearity for the four analytes was calculated from 5.0 to 50.0 μg kg−1. The decision limits (CCα) ranged from 6.2 to 6.4 μg kg−1 and from 6.1 to 6.5 μg kg−1 for honey and royal jelly, respectively. Detection capabilities values (CCβ) ranged between 7.2 and 7.7 μg kg−1 and from 7.3 to 7.9 μg kg−1 respectively for honey and royal jelly. The developed method is currently in use for confirmation of the official control
analysis of honey and royal jelly samples. 相似文献
18.
A multiresidue method has been developed for the simultaneous determination of sulfadiazine, sulfathiazole, sulfapyridine,
sulfamerazine, sulfamethoxydiazine, sulfamethylthiazole, sulfamethazine, sulfamonomethoxine, sulfamethoxypyridazine, sulfisoxazole,
sulfamethoxazole, sulfadimethoxine and sulfaquinoxaline in natural animal casings by HPLC after solid-phase extraction. The
sulfonamides were extracted with acetonitrile and the extract cleaned up with an Oasis MCX SPE cartridge prior to analysis.
Separation was on a ZOBAX Eclipse XDB-C8 column using gradient elution with acetonitrile/methanol/0.1% acetic acid. The effect of separation conditions on chromatographic
behavior and recovery has been studied. Calibration graphs were linear with very good correlation coefficients (r = 0.9983−0.9996) in the concentration range from 0.02 to 1 μg mL−1. The limits of quantitation (LOQ) for the 13 sulfonamides were in the range of 1.5–2.2 μg kg−1. Decision limits (CCα) and detection capabilities (CCβ) were in the range of 105.2–111.0 and 113.0–120.2 μg kg−1, respectively. The recovery for casings spiked with 1.5–100 μg kg−1 ranged from 65.2 to 85.9%. The relative standard deviations (RSDs) of the sulfonamides for six measurements at 100 μg kg−1 were from 2.2 to 7.7%. The applicability of the method to the analysis of salted swine casings, salted sheep casings and
dry casing samples was demonstrated. 相似文献
19.
Guillamont EM Lino CM Baeta ML Pena AS Silveira MI Vinuesa JM 《Analytical and bioanalytical chemistry》2005,383(4):570-575
Ochratoxin A (OTA) is a secondary fungal metabolite produced by several moulds, mainly by Aspergillus ochraceus and by Penicillium verrucosum, that occurs in meat products. The aim of this work was to optimize an efficient extraction procedure for the determination
of OTA in muscle tissue in order to assess its occurrence in meat samples. Three different apparatus, a Waring blender, a
switching apparatus, and an ultrasonic processor, were evaluated to verify the efficiency of extraction. The analytical methods
proposed involve the extraction with chloroform-orthophosphoric acid, cleanup through an immunoaffinity column, high-performance
liquid chromatography/fluorescence detection for separation and identification of OTA, and confirmation with liquid chromatography/FD
after methylation of OTA in muscle tissue. The limit of quantification of the proposed method was 0.04 μg kg−1. Recoveries of OTA, using switching apparatus, ranged from 90.3 to 103.2% for chicken muscle spiked at 2.4 and 0.48 μg kg−1, respectively, with a within-day relative standard deviation of 17 and 15.3%. The proposed method was applied to 38 chicken,
swine, and turkey muscle samples and the presence of OTA was confirmed in five samples. Finally, the estimated daily intake
of OTA in this study was between 23 pg kg−1 body weight per day for swine samples and 18 pg kg−1 body weight per day for turkey samples. 相似文献
20.
Liu X Xu J Li Y Dong F Li J Song W Zheng Y 《Analytical and bioanalytical chemistry》2011,399(7):2539-2547
A sensitive and effective method for simultaneous determination of triazolopyrimidine sulfonamide herbicide residues in soil,
water, and wheat was developed using ultra-performance liquid chromatography coupled with tandem mass spectrometry. The four
herbicides (pyroxsulam, flumetsulam, metosulam, and diclosulam) were cleaned up with an off-line C18 SPE cartridge and detected
by tandem mass spectrometry using an electrospray ionization source in positive mode (ESI+). The determination of the target
compounds was achieved in <2.0 min. The limits of detection were below 1 μg kg−1, while the limits of quantification did not exceed 3 μg kg−1 in different matrices. Quantitation was determined from calibration curves of standards containing 0.05–100 μg L−1 with r
2 > 0.997. Recovery studies were conducted at three spiked levels (0.2, 1, and 5 μg kg−1 for water; 5, 10, and 100 μg kg−1 for soil and wheat). The overall average recoveries for this method in water, soil, wheat plants, and seeds at three levels
ranged from 75.4% to 106.0%, with relative standard deviations in the range of 2.1–12.5% (n = 5) for all analytes. 相似文献