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1.
Boroujerdi AF Lee PA DiTullio GR Janech MG Vied SB Bearden DW 《Analytical and bioanalytical chemistry》2012,403(3):777-784
In-line solid-phase extraction–capillary electrophoresis coupled with mass spectrometric detection (SPE–CE–MS) has been used
for determination of 2-ethylidene-1,5-dimethyl-3,3-diphenylpyrrolidine (EDDP), codeine (COD), hydrocodeine (HCOD), and 6-acetylmorphine
(6AM) in urine. The preconcentration system consists of a small capillary filled with Oasis HLB sorbent and inserted into
the inlet section of the electrophoresis capillary. The SPE–CE–MS experimental conditions were optimized as follows: the sample
(adjusted to pH 6.0) was loaded at 930 mbar for 60 min, elution was performed with methanol at 50 mbar for 35 s, 60 mmol L−1 ammonium acetate at pH 3.8 was used as running buffer, the separation voltage was 30 kV, and the sheath liquid at a flow
rate of 5.0 μL min−1 was isopropanol–water 50:50 (v/v) containing 0.5% acetic acid. Analysis of urine samples spiked with the four drugs and diluted 1:1 (v/v) was studied in the linear range 0.08–10 ng mL−1. Detection limits (LODs) (S/N = 3) were between 0.013 and 0.210 ng mL−1. Repeatability (expressed as relative standard deviation) was below 7.2%. The method developed enables simple and effective
determination of these drugs of abuse in urine samples at the levels encountered in toxicology and doping. 相似文献
2.
Consuelo Cháfer-Pericás Ángel Maquieira Rosa Puchades Javier Miralles Amelia Moreno 《Analytical and bioanalytical chemistry》2010,396(2):911-921
An indirect competitive enzyme-linked immunosorbent assay (ELISA) was developed in plate to detect three sulfonamide residues
(sulfamerazine (SMR), sulfadimetoxine (SDM), and sulfadiazine (SDZ)) in gilthead sea bream (Sparus aurata) samples. Different extraction methodologies—using methanol/water 1:1 (v/v) + ethylene diamine tetraacetic acid (EDTA) 0.5% (m/v), acetonitrile, phosphate-buffered saline (PBS) 10 mmol L−1 pH 7 and acetate buffer 100 mmol L−1 pH 5—and cleanup steps, based on solid-phase extraction (C18, SCX, Si) or liquid extraction with hexane, were assayed. As optimum, a fast and simple method using acetonitrile was selected
to extract the sulfonamide residues from the edible muscle of fish. Due to matrix effects, a standard addition calibration
curve in fish extract is necessary for quantification purposes. Sulfonamide-free samples were spiked at different concentration
levels (between 30 and 90 ng g−1, 5–15 ng mL−1 in plate) and average recoveries (n = 8), ranging from 71% to 95%, 65% to 79%, and 72% to 95%, were obtained for SMR, SDM, and SDZ, respectively. The assay detection
limits for these antibiotics were lower than 100 μg kg−1 (maximum residue level established by the European Union). The accuracy was evaluated by spiking blank fish extracts at different
concentrations (10–40 ng mL−1, 5–20 ng mL−1 in plate), and the relative errors ranged between ±20%. Finally, in order to confirm the utility of the developed ELISA as
a screening methodology, fish samples from different supermarkets were analyzed, and results were compared with those obtained
by a validated high-performance liquid chromatography (HPLC) method. The correlation between the results obtained by both
ELISA and HPLC methods is satisfactory.
相似文献
3.
Zhao J Han X Zhao X Wang C Li Q Chen X Bi K 《Analytical and bioanalytical chemistry》2011,401(1):289-296
A liquid chromatographic–mass spectrometric (LC–MS) method has been developed and validated for simultaneous determination
of dehydroevodiamine and limonin from Evodia rutaecarpa in rat plasma. After addition of the internal standard, domperidone, plasma samples were extracted by liquid–liquid extraction
with ethyl acetate and separated on an Apollo C18 column (250 mm × 4.6 mm, 5 μm), with methanol–0.01% formic acid water (60:40, v/v) as mobile phase, within a runtime of 12.0 min. The analytes were detected without interference in the selected ion monitoring
(SIM) mode with positive electrospray ionization. The linear range was 1.0–500 ng mL−1 for dehydroevodiamine and 2.0–1,000 ng mL−1 for limonin, with lower limits of quantitation of 1.0 and 2.0 ng mL−1, respectively. Intra-day and inter-day precision were within 6.0% and 10.9%, respectively, for both analytes, and the accuracy
(relative error, RE, %) was less than 4.8% and 6.5%, respectively. The validated method was successfully applied to a comparative
pharmacokinetic study of dehydroevodiamine and limonin in rat plasma after oral administration of dehydroevodiamine, limonin,
and an aqueous extract of Evodiae fructus. The results indicated there were obvious differences between the pharmacokinetic behavior after oral administration of an
aqueous extract of Evodiae fructus compared with single substances. 相似文献
4.
Vitor RV Martins MC Figueiredo EC Martins I 《Analytical and bioanalytical chemistry》2011,400(7):2109-2117
A method constituted by molecularly imprinted solid-phase extraction (MISPE) with high-performance liquid chromatography coupled
to diode array detector (HPLC-DAD) was developed for cotinine analysis in saliva samples. For this purpose, the separation
was carried out with a C18 reversed-phase column at 20 °C. The mobile phase which was composed of a mixture of 09:91 (v/v) acetonitrile/phosphate buffer, pH 6.3, was delivered with isocratic flow rate at 1.4 mL min−1. Employing MISPE, the best conditions were achieved with 1.5 mL of saliva plus 1.5 mL of 0.1 mol L−1 of acetate buffer, pH 5.5, which were then passed through a cartridge previously conditioned with 2 mL acetonitrile, 2 mL
methanol, and 2 mL of 0.1 mol L−1 sodium acetate buffer, pH 5.5. The washing was carried out with 1 mL deionized water, 1 mL of 0.1 mol L−1 sodium hydroxide, and 1 mL hexane; finally; the cotinine elution was carried out with 3 mL methanol/water (97.5: 2.5, v/v). Linearity ranged from 30 to 500 ng mL−1 with r > 0.99. Intra-assay, interassay precision, and accuracy ranged from 3.1% to 10.1%, 5.2% to 15.9%, and 99.22% to 111.17%,
respectively. The detection and quantification limits were 10 and 30 ng mL−1, respectively. This investigation has provided a reliable method for routine cotinine determination in saliva, and it is
an important tool for monitoring cigarette smoke exposure in smokers. The method was applied in five smokers’ samples who
consumed around five to 20 cigarettes per day and the values of cotinine in saliva were from 66.7 to 316.16 ng mL−1. 相似文献
5.
Ming-Zhou Zhang Min-Zi Wang Zong-Lun Chen Jie-Hong Fang Mei-Ming Fang Jun Liu Xiao-Ping Yu 《Analytical and bioanalytical chemistry》2009,395(8):2591-2599
A multianalyte lateral-flow immunochromatographic technique using colloidal gold-labeled polyclonal antibodies was developed
for the rapid simultaneous detection of clenbuterol and ractopamine. The assay procedure could be accomplished within 5 min,
and the results of this qualitative one-step assay were evaluated visually according to whether test lines appeared or not.
When applied to the swine urines, the detection limit and the half maximal inhibitory concentration (IC50) of the test strip under an optical density scanner were calculated to be 0.1 ± 0.01 ng mL−1 and 0.1 ± 0.01 ng mL−1, 0.56 ± 0.08 ng mL−1, and 0.71 ± 0.06 ng mL−1, respectively, the cut-off levels with the naked eye of 1 ng mL−1 and 1 ng mL−1 for clenbuterol and ractopamine were observed. Parallel analysis of swine urine samples with clenbuterol and ractopamine
showed comparable results obtained from the multianalyte lateral-flow test strip and GC-MS. Therefore, the described multianalyte
lateral-flow test strip can be used as a reliable, rapid, and cost-effective on-site screening technique for the simultaneous
determination of clenbuterol and ractopamine residues in swine urine.
相似文献
6.
CdTe quantum dots (QDs) were modified with thioglycolic acid (TGA) and synthesized in aqueous medium. The optimum fluorescence
intensity was found to be at pH 6.24 with a CdTe QDs concentration of 4.96 × 10−7 mol L−1. The quenched fluorescence intensity of CdTe QDs is linearly proportional to V(V) concentration from 10 to 200 ng mL−1 with correlation coefficient R = 0.9985. The limit of detection for V(V) was 2.07 ng mL−1. The proposed method was successfully applied to the analysis of trace amounts of V(V) in water samples with recovery of
96.5–101.8%, and the results were in good agreement with those of electrothermal atomic absorption spectrometry. 相似文献
7.
Borges KB de Oliveira AR Barth T Jabor VA Pupo MT Bonato PS 《Analytical and bioanalytical chemistry》2011,399(2):915-925
The purpose of this study was the development and validation of an LC–MS–MS method for simultaneous analysis of ibuprofen
(IBP), 2-hydroxyibuprofen (2-OH-IBP) enantiomers, and carboxyibuprofen (COOH-IBP) stereoisomers in fungi culture medium, to
investigate the ability of some endophytic fungi to biotransform the chiral drug IBP into its metabolites. Resolution of IBP
and the stereoisomers of its main metabolites was achieved by use of a Chiralpak AS-H column (150 × 4.6 mm, 5 μm particle
size), column temperature 8 °C, and the mobile phase hexane–isopropanol–trifluoroacetic acid (95: 5: 0.1, v/v) at a flow rate of 1.2 mL min−1. Post-column infusion with 10 mmol L−1 ammonium acetate in methanol at a flow rate of 0.3 mL min−1 was performed to enhance MS detection (positive electrospray ionization). Liquid–liquid extraction was used for sample preparation
with hexane–ethyl acetate (1:1, v/v) as extraction solvent. Linearity was obtained in the range 0.1–20 μg mL−1 for IBP, 0.05–7.5 μg mL−1 for each 2-OH-IBP enantiomer, and 0.025–5.0 μg mL−1 for each COOH-IBP stereoisomer (r ≥ 0.99). The coefficients of variation and relative errors obtained in precision and accuracy studies (within-day and between-day)
were below 15%. The stability studies showed that the samples were stable (p > 0.05) during freeze and thaw cycles, short-term exposure to room temperature, storage at −20 °C, and biotransformation
conditions. Among the six fungi studied, only the strains Nigrospora sphaerica (SS67) and Chaetomium globosum (VR10) biotransformed IBP enantioselectively, with greater formation of the metabolite (+)-(S)-2-OH-IBP. Formation of the COOH-IBP stereoisomers, which involves hydroxylation at C3 and further oxidation to form the
carboxyl group, was not observed. 相似文献
8.
A new procedure is described for the derivatization by silylation of 11-nor-Δ9-tetrahydrocannabinol-9-carboxylic acid (THCCOOH) present in urine, followed by analysis using gas chromatography–tandem mass
spectrometry. A conventional procedure for derivatization of the analyte was evaluated using two types of experimental design.
A 23 factorial design considered the parameters temperature, reaction time, and the solvent/derivatization agent ratio. A central
composite design (CCD) was applied to optimize the values of the significant variables. The optimum conditions were a reaction
temperature of 50 °C, a reaction time of 30 min, and a BSTFA/acetone ratio of 40:20. The use of imidazole as a catalyst, together
with ultrasonication, reduced the reaction time to 5 min and increased the efficiency of derivatization of THCCOOH, compared
with the conventional method. The operating conditions of the tandem mass spectrometer were also optimized. The method was
linear in the concentration range 1–50 ng mL−1 (R
2 = 0.9951). Intra- and inter-day precisions were 7.7–12.3% and 11.1–13.9%, respectively, recoveries ranged between 91 ± 8%
and 101 ± 12%, accuracy (as % bias) was between –11.7% and +0.7%, and limits of detection and quantification were 0.5 and
1.0 ng mL−1, respectively. 相似文献
9.
Bagheri H Aghakhani A Akbari M Ayazi Z 《Analytical and bioanalytical chemistry》2011,400(10):3607-3613
A micro-solid phase extraction technique was developed using a novel polypyrrole-polyamide nanofiber sheet, fabricated by
electrospinning method. The applicability of the new nanofiber sheet was examined as an extracting medium to isolate malathion
as a model pesticide from aqueous samples. Solvent desorption was subsequently performed in a microvial, and an aliquot of
extractant was injected into gas chromatography–mass spectrometry. Various parameters affecting the electrospinning process
including monomer concentration, polyamide content, applied voltage, and electrospinning time were examined. After fabricating
the most suitable preparation conditions, influential parameters on the extraction and desorption processes were optimized.
The developed method proved to be rather convenient and offers sufficient sensitivity and good reproducibility. The limit
of detection (S/N = 3) and limit of quantification (S/N = 10) of the method under optimized conditions were 50 and 100 ng L−1, respectively. The relative standard deviation at concentration level of 1 ng mL−1 was 2% (n = 3). The calibration curve of analyte showed linearity in the range of 0.1–1 ng mL−1 (R
2 = 0.9975). The developed method was successfully applied to tap and Zayanderood river water samples, while the relative recovery
percentages of 98% and 96% were obtained, respectively. The whole procedure showed to be conveniently applicable and quite
easy to be manipulated. 相似文献
10.
Benito-Peña E Martins S Orellana G Moreno-Bondi MC 《Analytical and bioanalytical chemistry》2009,393(1):235-245
A novel water-compatible molecularly imprinted polymer (MIP), prepared with enrofloxacin (ENR) as the template, has been optimised
for the selective extraction of fluoroquinolone antibiotics in aqueous media. The results of a morphological characterisation
and selectivity tests of the polymer material for ENR and related derivatives are reported. High affinity for the piperazine-based
fluoroquinolones marbofloxacin, ciprofloxacin, norfloxacin and ofloxacin was observed, whereas no retention was found for
nonrelated antibiotics. Various parameters affecting the extraction efficiency of the polymer have been optimised to achieve
selective extraction of the antibiotics from real samples and to reduce nonspecific interactions. These findings resulted
in a MISPE/HPLC-FLD method allowing direct extraction of the analytes from aqueous samples with a selective wash using just
50% (v/v) organic solvent. The method showed excellent recoveries and precision when buffered urine samples fortified at five
concentration levels (25–250 ng mL−1 each) of marbofloxacin, ciprofloxacin, norfloxacin, enrofloxacin and sarafloxacin were tested (53–88%, RSD 1–10%, n = 3). Moreover, the biological matrix of the aqueous samples did not influence the preconcentration efficiency of the fluoroquinolones
on the MIP cartridges; no significant differences were observed between the recovery rates of the antibiotics in buffer and
urine samples. The detection limits of the whole process range between 1.9 and 34 ng mL–1 when 5-mL urine samples are processed. The developed method has been successfully applied to preconcentration of norfloxacin
in urine samples of a medicated patient, demonstrating the ability of the novel MIP for selective extraction of fluoroquinolones
in urine samples. 相似文献
11.
Viñas P López-García I Bravo-Bravo M Briceño M Hernández-Córdoba M 《Analytical and bioanalytical chemistry》2012,403(4):1059-1066
A miniaturized dispersive liquid–liquid microextraction (DLLME) procedure coupled to liquid chromatography (LC) with fluorimetric
detection was evaluated for the preconcentration and determination of thiamine (vitamin B1). Derivatization was carried out by chemical oxidation of thiamine with 5 × 10−5 M ferricyanide at pH 13 to form fluorescent thiochrome. For DLLME, 0.5 mL of acetonitrile (dispersing solvent) containing
90 μL of tetrachloroethane (extraction solvent) was rapidly injected into 10 mL of sample solution containing the derivatized
thiochrome and 24% (w/v) sodium chloride, thereby forming a cloudy solution. Phase separation was carried out by centrifugation, and a volume of
20 μL of the sedimented phase was submitted to LC. The mobile phase was a mixture of a 90% (v/v) 10 mM KH2PO4 (pH 7) solution and 10% (v/v) acetonitrile at 1 mL min−1. An amide-based stationary phase involving a ligand with amide groups and the endcapping of trimethylsilyl was used. Specificity,
linearity, precision, recovery, and sensitivity were satisfactory. Calibration graph was carried out by the standard additions
method and was linear between 1 and 10 ng mL−1. The detection limit was 0.09 ng mL−1. The selectivity of the method was judged from the absence of interfering peaks at the thiamine elution time for blank chromatograms
of unspiked samples. A relative standard deviation of 3.2% was obtained for a standard solution containing thiamine at 5 ng mL−1. The esters thiamine monophosphate and thiamine pyrophosphate can also be determined by submitting the sample to successive
acid and enzymatic treatments. The method was applied to the determination of thiamine in different foods such as beer, brewer’s
yeast, honey, and baby foods including infant formulas, fermented milk, cereals, and purees. For the analysis of solid samples,
a previous extraction step was applied based on an acid hydrolysis with trichloroacetic acid. The reliability of the procedure
was checked by analyzing a certified reference material, pig’s liver (CRM 487). The value obtained was 8.76 ± 0.2 μg g−1 thiamine, which is in excellent agreement with the certified value, 8.6 ± 1.1 μg g−1. 相似文献
12.
Akhmad Sabarudin Osamu Noguchi Mitsuko Oshima Keiro Higuchi Shoji Motomizu 《Mikrochimica acta》2007,159(3-4):341-348
Chitosan resin functionalized with 3,4-dihydroxy benzoic acid (CCTS-DHBA resin) was used as a packing material for flow injection
(FI) on-line mini-column preconcentration in combination with inductively coupled plasma-atomic emission spectrometry (ICP-AES)
for the determination of trace elements such as silver, bismuth, copper, gallium, indium, molybdenum, nickel, uranium, and
vanadium in environmental waters. A 5-mL aliquot of sample (pH 5.5) was introduced to the minicolumn for the adsorption/preconcentration
of the metal ions, and the collected analytes on the mini-column were eluted with 2 M HNO3, and the eluates was subsequently transported via direct injection to the nebulizer of ICP-AES for quantification. The parameters
affecting on the sensitivity, such as sample pH, sample flow rate, eluent concentration, and eluent flow rate, were carefully
examined. Alkali and alkaline earth metal ions commonly existing in river water and seawater did not affect the analysis of
metals. Under the optimum conditions, the method allowed the determination of metal ions with detection limits of 0.08 ng mL−1 (Ag), 0.9 ng mL−1 (Bi), 0.07 ng mL−1 (Cu), 0.9 ng mL−1 (Ga), 0.9 ng mL−1 (In), 0.08 ng mL−1 (Mo), 0.09 ng mL−1 (Ni), 0.9 ng mL−1 (U), and 0.08 ng mL−1 (V). By using 5 mL of sample solution, the enrichment factor and collection efficiency were 8–12 fold and 96–102%, respectively,
whereas the sample throughput was 7 samples/hour. The method was validated by determining metal ions in certified reference
material of river water (SLRS-4) and nearshore seawater (CASS-4), and its applicability was further demonstrated to river
water and seawater samples. 相似文献
13.
A rapid, ultra high-performance liquid chromatographic (UHPLC) method has been developed and validated for simultaneous identification
and analysis of the isoflavones genistein, daidzein, glycitin, puerarin, and biochanin A, and the flavonoids (±)-catechin,
(−)-epicatechin, rutin, hesperidin, neohesperidin, quercitrin, and hesperetin in human urine. Urine samples were incubated
with β-glucuronidase/sulfatase. UHPLC was performed with a Hypersil Gold (50 × 2.1 mm, 1.9 μm) analytical column. Elution
was with a gradient prepared from aqueous trifluoroacetic acid (0.05%) and acetonitrile. UV detection was performed at 254
and 280 nm. The calibration curves were indicative of good linearity (r
2 ≥ 0.9992) in the range of interest for each analyte. LODs ranged between 15.4 and 107.0 ng mL−1 and 3.9 and 20.4 ng mL−1 for flavonoids and isoflavones, respectively. Intra-day and inter-day precision (C.V., %) was less than 3.9% and 3.8%, respectively,
and accuracy was between 0.03% and 5.0%. Recovery was 70.35–96.58%. The method is very rapid, simple, and reliable, and suitable
for pharmacokinetic analysis. It can be routinely used for simultaneous determination of these five isoflavones and seven
flavonoids in human urine. The method can also be applied to studies after administration of pharmaceutical preparations containing
isoflavones and flavonoids to humans. 相似文献
14.
A fast and sensitive liquid chromatography–mass spectrometry method was developed for the determination of ursolic acid (UA)
in rat plasma and tissues. Glycyrrhetinic acid was used as the internal standard (IS). Chromatographic separation was performed
on a 3.5 μm Zorbax SB-C18 column (30 mm × 2.1 mm) with a mobile phase consisting of methanol and aqueous 10 mM ammonium acetate
using gradient elution. Quantification was performed by selected ion monitoring with (m/z)− 455 for UA and (m/z)− 469 for the IS. The method was validated in the concentration range of 2.5 − 1470 ng mL−1 for plasma samples and 20 − 11760 ng g−1 for tissue homogenates. The intra- and inter-day assay of precision in plasma and tissues ranged from 1.6% to 7.1% and 3.7%
to 9.0%, respectively, and the intra- and inter-day assay accuracy was 84.2 − 106.9% and 82.1 − 108.1%, respectively. Recoveries
in plasma and tissues ranged from 83.2% to 106.2%. The limits of detections were 0.5 ng mL−1 or 4.0 ng g−1. The recoveries for all samples were >90%, except for liver, which indicated that ursolic acid may metabolize in liver. The
main pharmacokinetic parameters obtained were T
max = 0.42 ± 0.11 h, C
max = 1.10 ± 0.31 μg mL−1, AUC = 1.45 ± 0.21 μg h mL−1 and K
a = 5.64 ± 1.89 h−1. The concentrations of UA in rat lung, spleen, liver, heart, and cerebellum were studied for the first time. This method
is validated and could be applicable to the investigation of the pharmacokinetics and tissue distribution of UA in rats. 相似文献
15.
Cooper EM Covaci A van Nuijs AL Webster TF Stapleton HM 《Analytical and bioanalytical chemistry》2011,401(7):2123-2132
Organophosphate triesters tris(1,3-dichloro-2-propyl) phosphate (TDCPP) and triphenyl phosphate are widely used flame retardants
(FRs) present in many products common to human environments, yet understanding of human exposure and health effects of these
compounds is limited. Monitoring urinary metabolites as biomarkers of exposure can be a valuable aid for improving this understanding;
however, no previously published method exists for the analysis of the primary TDCPP metabolite, bis(1,3-dichloro-2-propyl)
phosphate (BDCPP), in human urine. Here, we present a method to extract the metabolites BDCPP and diphenyl phosphate (DPP)
in human urine using mixed-mode anion exchange solid phase extraction and mass-labeled internal standards with analysis by
atmospheric pressure chemical ionization liquid chromatography tandem mass spectrometry. The method detection limit was 8 pg mL−1 urine for BDCPP and 204 pg mL−1 for DPP. Recoveries of analytes spiked into urine ranged from 82 ± 10% to 91 ± 4% for BDCPP and from 72 ± 12% to 76 ± 8%
for DPP. Analysis of a small number of urine samples (n = 9) randomly collected from non-occupationally exposed adults revealed the presence of both BDCPP and DPP in all samples.
Non-normalized urinary concentrations ranged from 46–1,662 pg BDCPP mL−1 to 287–7,443 pg DPP mL−1, with geometric means of 147 pg BDCPP mL−1 and 1,074 pg DPP mL−1. Levels of DPP were higher than those of BDCPP in 89% of samples. The presented method is simple and sufficiently sensitive
to detect these FR metabolites in humans and may be applied to future studies to increase our understanding of exposure to
and potential health effects from FRs. 相似文献
16.
A sensitive chemiluminescence method for the determination of clindamycin is presented. The method is based on the inhibitory
effect of clindamycin on the chemiluminescence reaction between luminol and myoglobin in a flow-injection system. The decrement
in chemiluminescence intensity is linear with the logarithm of the clindamycin concentration over the range of 0.1–70.0 ng mL−1 (r
2 = 0.9995), with a detection limit of 0.03 ng mL−1 (3σ). At a flow rate of 2.0 mL min−1, the complete analytical process could be performed within 0.5 min, including sampling and washing, with a relative standard
deviation of less than 3.0% (n = 5). The procedure was applied to the determination of clindamycin in human serum and in monitoring
the excretion of clindamycin in human urine samples without any pretreatment process. It was found that the excretive clindamycin
concentration reached its maximum 3 hours after oral administration. The clindamycin excretive ratio in 9 hours was 10.84%
in the body of the volunteer. 相似文献
17.
Simple and rapid fluorometric screening methods have been developed based on the competitive binding between the target and
an intercalating fluorophore dye to double-stranded-DNA (dsDNA). In this study, the long-wavelength fluorescente dye TOTO-3
was employed as the indicator. Compounds that interact with dsDNA will affect the binding of TOTO-3 to the nucleic acid thereby
changing the fluorescence intensity. The analyte concentration is indirectly determined by the decrease in fluorescence intensity.
A fiber optic fluorescence screening system was developed for rapid and convenient sample processing. Lambda DNA (48.5 kb)
was chosen as a suitable sensing nucleic acid material. Detection of sulfathiazole and chloramphenicol in shrimps using this
method was studied in the range of 0.5–25 ng mL−1 of sulfathiazole and of 1–50 ng mL−1 of chloramphenicol. Detection limits of 0.5 ng mL−1 of sulfathiazole and 1 ng mL−1 of chloramphenicol were achieved. This approach is useful as a routine test in the monitoring of antibiotics in the environment
or aquaculture products. The easy operation and the rapid and sensitive detection make this a potential high-throughput screening
method. 相似文献
18.
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
19.
Xu Y Wang C Zhang X Chen H Zhao Q Song W Wang H Zeng Q Ding L 《Analytical and bioanalytical chemistry》2011,400(2):517-526
In the study, a fast and selective method based on magnetic separation has been developed for the extraction of nicotine from
human plasma using magnetic strong cation exchange (MSCX) resins as adsorbent. MSCX resins were prepared using hydrophobic
Fe3O4 magnetite as magnetically susceptible component, styrene and acrylic acid as polymeric matrix components, and acetyl sulfonate
as the sulfonation agent. The extraction procedure was carried out in a single step by stirring the mixture of diluted plasma
sample and MSCX resins in the vortex for 5 min. Then, the resins with adsorbed nicotine were separated from the sample matrix
by applying an appropriate magnetic field. Main factors affecting the extraction of nicotine such as the amount of MSCX resins,
pH value of the extraction solvent, extraction time, and washing and eluting conditions were optimized. The nicotine eluted
from the resins was determined by liquid chromatography–tandem mass spectrometry. The calibration curve obtained by analyzing
matrix-matched standards shows excellent linear relationship (r
2 = 0.9998) in the concentration range of 10–2,500 ng mL−1. The limit of detection and quantification obtained are 2.9 and 9.7 ng mL−1, respectively. The relative standard deviations of intra- and inter-day obtained are in the range of 1.9–6.9% and 2.5–7.8%
with the recoveries ranging from 78.7% to 99.1%. The proposed method was successfully applied to determine nicotine in human
plasma phlebotomized from ten male smokers. Nicotine was detectable with the contents ranging from 44.4 to 221.9 ng mL−1 in five samples. 相似文献
20.
A novel method for the determination of proteins at nanogram levels was proposed based on the decrease of resonance light
scattering (RLS) signal resulting from the interaction of dibromo-o-nitrophenylfluorone (DBONPF)-sodium lauroyl glutamate
(SLG) with proteins. At pH 2.97, the decrease RLS intensity was proportional to the concentration of proteins in the range
of nanogram levels with 3σ detection limits being 3.4 ng mL−1 for bovine serum albumin (BSA), 1.7 ng mL−1 for human serum albumin (HSA), 4.1 ng mL−1 for γ-globulin (γ-IgG), 4.4 ng mL−1 for egg albumin, 6.2 ng mL−1 for pepsin (Pep) and 3.7 ng mL−1 for α-chymotrypsin (Chy). The method is no protein-to-protein variability, simple, rapid, practical and relatively free
from interference from coexisting substance, as well as much more sensitive than most of the reported methods. The proposed
method was successfully applied to determine total protein in human serum samples. 相似文献