共查询到20条相似文献,搜索用时 593 毫秒
1.
Naoya Kishikawa Nobuhiro Ohkubo Kaname Ohyama Kenichiro Nakashima Naotaka Kuroda 《Analytical and bioanalytical chemistry》2009,393(4):1337-1343
A sensitive and selective chemiluminescence assay for the determination of quinones was developed. The method was based on
generation of reactive oxygen species through the redox reaction between quinone and dithiothreitol as reductant, and then
the generated reactive oxygen was detected by luminol chemiluminescence. The chemiluminescence was intense, long-lived, and
proportional to quinone concentration. It is concluded that superoxide anion was involved in the proposed chemiluminescence
reaction because the chemiluminescence intensity was decreased only in the presence of superoxide dismutase. Among the tested
quinones, the chemiluminescence was observed from 9,10-phenanthrenequinone, 1,2-naphthoquinone, and 1,4-naphthoquinone, whereas
it was not observed from 9,10-anthraquinone and 1,4-benzoquinone. The chemiluminescence property was greatly different according
to the structure of quinones. The chemiluminescence was also observed for biologically important quinones such as ubiquinone.
Therefore, a simple and rapid assay for ubiquinone in pharmaceutical preparation was developed based on the proposed chemiluminescence
reaction. The detection limit (blank + 3SD) of ubiquinone was 0.05 μM (9 ng/assay) with an analysis time of 30 s per sample.
The developed assay allowed the direct determination of ubiquinone in pharmaceutical preparation without any purification
procedure.
Figure Chemiluminescence generated through the redox cycle of quinone 相似文献
2.
Khalid Hamad Abu-Shandi 《Analytical and bioanalytical chemistry》2009,395(2):527-532
A high-performance liquid chromatographic (HPLC) method with fluorescence detection for the quantification of vancomycin in
human plasma was developed and validated. The method includes an extraction of vancomycin by deproteinization with acetonitrile.
The analyses were carried out at 258 nm as the emission wavelength while exciting at 225 nm on a reversed-phase column (30 cm × 4 mm
i.d. × 10 μm Waters Associates μBondapak C18) using a mobile phase composed of methanol and phosphate buffer at pH 6.3. Vancomycin
was quantitatively recovered from human plasma samples (>96%) with high values of precision. The separation was completed
within 27 min. The calibration curve was linear over the range from 5 to 1,000 ng/mL with the detection and quantification
limits of 2 ng/mL and 5 ng/mL, respectively. This method is suitable for the routine assay of plasma samples.
Figure The effect of the deproteinization solvent on the signal of the interference peak at retention time of 15.0 min. The peak
which interferes with the peaks of Erythromycin and Vancomycin has been disappeared by using 2 mL acetonitrile as the deproteinization
solvent. 相似文献
3.
Takeshi Kumazawa Koichi Saeki Isao Yanagisawa Seisaku Uchigasaki Chika Hasegawa Hiroshi Seno Osamu Suzuki Keizo Sato 《Analytical and bioanalytical chemistry》2009,394(4):1161-1170
This paper describes a fully automated on-line method combining in-tube solid-phase microextraction (SPME) in which sample
clean-up and enrichment are conducted through an open tubular fused-silica capillary column and high-performance liquid chromatography
(HPLC)/tandem mass spectrometry (MS/MS) detection for the determination of six butyrophenone derivatives (moperone, floropipamide,
haloperidol, spiroperidol, bromperidol, and pimozide) in human plasma samples. The six butyrophenones were extracted by repeatedly
aspirating and dispensing plasma sample solutions on a DB-17 capillary column (60 cm × 0.32 mm i.d., film thickness 0.25 μm).
The analytes retained on the inner surface of the capillary column were then eluted into an acetonitrile-rich mobile phase
using a gradient separation technique. Extraction efficiencies ranged from 12.7% to 31.8% for moperone, spiroperidol, and
pimozide, and from 1.08% to 4.86% for floropipamide, haloperidol, and bromperidol. The regression equations for all compounds
showed excellent linearity, ranging from 0.05 to 50 ng/0.1 mL of plasma, except for moperone and spiroperidol (0.01 to 50 ng/0.1 mL).
The limits of detection and quantification in plasma for each drug were 0.03–0.2 and 0.1–0.5 ng/mL, respectively. The intra-
and inter-day coefficients of variation for all compounds in plasma were not greater than 13.7%. 相似文献
4.
A liquid chromatography–chemiluminescence detection method was developed and validated for the determination of catecholamines
(norepinephrine, epinephrine, and dopamine) in mouse brains. Chromatography was performed on a strong cation exchange column
(150 × 2.0-mm id) using an isocratic mobile phase of 65 mM potassium acetate/75 mM potassium phosphate (95:5, pH 3.5) at a
flow rate of 0.2 mL/min following post-column fluorescence derivatization of catecholamines with ethylenediamine and peroxyoxalate
chemiluminescence reaction detection. The recovery of catecholamines added to mouse brain samples was more than 95.0%, while
intra- and inter-day precision of the assay were <4.8%. The validated method was used to determine norepinephrine and dopamine
concentrations in mouse brains without prior sample purification. 相似文献
5.
Lawrence Asamoah Adutwum Naoya Kishikawa Kaname Ohyama Shiro Harada Kenichiro Nakashima Naotaka Kuroda 《Analytical and bioanalytical chemistry》2010,398(2):823-829
A sensitive and selective high performance liquid chromatography-peroxyoxalate chemiluminescence (PO-CL) method has been developed
for the simultaneous determination of chlorpheniramine (CPA) and monodesmethyl chlorpheniramine (MDCPA) in human serum. The
method combines fluorescent labeling with 4-(4,5-diphenyl-1H-imidazole-2-yl)phenyl boronic acid using Suzuki coupling reaction with PO-CL detection. CPA and MDCPA were extracted from
human serum by liquid–liquid extraction with n-hexane. Excess labeling reagent, which interfered with trace level determination of analytes, was removed by solid-phase
extraction using a C18 cartridge. Separation of derivatives of both analytes was achieved isocratically on a silica column
with a mixture of acetonitrile and 60 mM imidazole-HNO3 buffer (pH 7.2; 85:15, v/v) containing 0.015% triethylamine. The proposed method exhibited a good linearity with a correlation coefficient of 0.999
for CPA and MDCPA within the concentration range of 0.5–100 ng/mL. The limits of detection (S/N = 3) were 0.14 and 0.16 ng/mL
for CPA and MDCPA, respectively. Using the proposed method, CPA could be selectively determined in human serum after oral
administration. 相似文献
6.
Hua Wei Jun Wen Rui Xie Houwen Lin Guorong Fan Yutian Wu 《Analytical and bioanalytical chemistry》2009,395(5):1461-1469
A sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method, followed by a 96-well protein precipitation,
has been developed and fully validated for the determination of Phakellistatin 13 (PK13), a new cyclic heptapeptide isolated
from the sponge Phakellia fusca Thiele, in rat plasma. After protein precipitation of the plasma samples (50 μL) in a 96-well plate by methanol (200 μL)
containing the internal standard Pseudostellarin B (20 ng/mL), the plate was vortex mixed for 3 min. Following filtration
for 5 min, the filtrate was directly injected into the LC-MS/MS system. The analytes were separated on an XB-C18 analytical
column (5 μm, 50 mm × 4.6 mm i.d.) using an eluent of methanol–water (85:15, v/v) and detected by electrospray ionization mass spectrometry in the negative multiple reaction monitoring mode with a chromatographic
run time of 5.0 min. The method was sensitive with a lower limit of quantification (LLOQ) of 0.1 ng/mL, with good linearity
(r > 0.999) over the quantitation range of 0.1–5 ng/mL. The validation results demonstrated that this method was significantly
specific, accurate, precise, and was successfully applied in measuring levels of PK13 in rat plasma following intravenous
administration of 20, 50, and 100 μg/kg of peptide in rats, respectively, which was suitable for the preclinical pharmacokinetic
studies on PK13. 相似文献
7.
A novel chemiluminescence method for the determination of levofloxacin is presented, which is based on the inhibitory effect
of levofloxacin on the chemiluminescence reaction between luminol and myoglobin in a flow-injection system. The decrement
of chemiluminescence intensity is linear with the logarithm of levofloxacin concentration over the range from 0.07 to 100.0
ng/mL (r
2 = 0.9994), with the detection limit of 0.02 ng/mL (3σ). At a flow rate of 2.0 mL/min, a 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 proposed procedure was applied successfully to the determination of levofloxacin in pharmaceutical preparations,
human urine and serum without any pretreatment procedure. 相似文献
8.
Fluorescence polarization immunoassay for rapid screening of ochratoxin A in red wine 总被引:1,自引:0,他引:1
Francesco Zezza Francesco Longobardi Michelangelo Pascale Sergei A. Eremin Angelo Visconti 《Analytical and bioanalytical chemistry》2009,395(5):1317-1323
A fluorescence polarization (FP) immunoassay, based on a monoclonal antibody and an ochratoxin A (OTA)-fluorescein tracer,
has been developed for rapid screening of OTA in red wine. Wine samples were diluted with methanol and passed through aminopropyl
solid-phase extraction columns prior to the FP assay. Average recoveries from samples spiked with OTA at levels of 2.0 and
5.0 ng/mL were 79% with RDS of 11% (n = 6). The limit of detection of the FP immunoassay was 0.7 ng/mL OTA, and the whole analysis was performed in less than 10 min.
The assay was tested on 154 red wine samples (naturally contaminated or spiked at level ranging from 0.1 to 5.0 ng/mL) and
compared with an high-performance liquid chromatography/immunoaffinity column clean-up method, showing a good correlation
(r = 0.9222). Their compliance with the European regulation (2.0 ng/mL OTA maximum permitted level) was correctly assessed for
70% of the analyzed samples of red wine, whereas confirmatory analyses were required for the remaining ones with OTA levels
close to the regulatory limit. No false-negative or positive results were observed using the FP immunoassay. The proposed
FP assay is a useful screening method for OTA in red wines, when high throughput is required, that could also be used for
white and rosé wines, which are known to contain less interfering compounds such as polyphenols. 相似文献
9.
Monterola MP Smith BW Omenetto N Winefordner JD 《Analytical and bioanalytical chemistry》2008,391(7):2617-2626
A simple, fast, reliable, sensitive and potentially portable explosive detection device was developed employing laser photofragmentation
(PF) followed by heterogeneous chemiluminescence (CL) detection. The PF process involves the release of NOx(x = 1,2) moieties from explosive compounds such as TNT, RDX, and PETN through a stepwise excitation–dissociation process using a 193 nm
ArF laser. The NOx(x = 1,2) produced upon PF is subsequently detected by its CL reaction with basic luminol solution. The intensity of the CL signal
was detected by a thermoelectrically cooled photomultiplier tube with high quantum efficiency and negligible dark current
counts. The system was able to detect trace amounts of explosives in various forms in real time under ambient conditions.
Detection limits of 3 ppbv for PETN, 2 ppbv for RDX, and 34 ppbv for TNT were obtained. It was also demonstrated that the
presence of PETN residue within the range of 61 to 186 ng/cm2 can be detected at a given signal-to-background ratio of 10 using a few microjoules of laser energy. The technique also demonstrated
its potential for the direct analysis of trace explosive in soil. An LOD range of 0.5–4.3 ppm for PETN was established, which
is comparable to currently available techniques.
Figure Photofragmentation–chemiluminescence detector 相似文献
10.
Carola W. N. Damen Hilde Rosing Jan H. M. Schellens Jos H. Beijnen 《Analytical and bioanalytical chemistry》2009,394(4):1171-1182
A sensitive, specific and efficient high-performance liquid chromatography-tandem mass spectrometry assay for the simultaneous
determination of vincristine and actinomycin-D in human dried blood spots is presented. Dried blood spots were punched out
of a collection paper with a 0.25-in.-diameter punch. The analytes were extracted from the punched-out disc using sonication
during 15 min in a mixture of acetonitrile–methanol–water (1:1:1, v/v/v) containing the internal standard vinorelbine. Twenty-microlitre volumes were injected onto the HPLC system. Separation was
achieved on a 50 × 2.1 mm ID Xbridge C18 column using elution with 1 mM ammonium acetate–acetonitrile (70:30, v/v) adjusted to pH 10.5 with ammonia and run in a gradient with methanol at a flow rate of 0.4 mL/min. HPLC run time was 6 min.
The assay quantifies vincristine from 1 to 100 ng/mL and actinomycine-D from 2 to 250 ng/mL using a blood sample obtained
by a simple finger prick. Validation results demonstrate that vincristine and actinomycin-D can be accurately and precisely
quantified in human dried blood spots with the presented method. The assay can now be used to support clinical pharmacologic
studies with vincristine and actinomycin-D. 相似文献
11.
A rapid flow-injection method with chemiluminescence (CL) detection is described for the determination of glutathione (GSH).
The method is based on the CL reaction of luminol and hydrogen peroxide. GSH can greatly enhance the chemiluminescence intensity
in 0.1 mol/L borax–sodium hydroxide buffer solution (pH = 9.7). The maximum CL intensity was directly proportional to the
concentration of GSH in the range 3.0 × 10−7–2.0 × 10−5 mol/L, and the detection limit was 6.8 × 10−8 mol/L. The relative standard deviation was 3.4% for 5.0 × 10−6 mol/L of GSH (n = 11).
Received October 23, 2001; accepted June 18, 2002 相似文献
12.
A sensitive chemiluminescence method based on enhancing the effect of cefetamet pivoxil on the chemiluminescent reaction between
luminol and dissolved oxygen in a flow injection system was proposed for the determination of cefetamet pivoxil. The increment
of the chemiluminescence intensity was proportional to the concentration of cefetamet pivoxil, which yields a calibration
graph that is linear over the concentration from 0.4 to 100.0 ng/mL (r
2 = 0.991) with the detection limit of 0.1 ng/mL (3σ). At a flow rate of 2.0 mL/min complete determination of cefetamet pivoxil,
including sampling and washing, could be accomplished in 40 s with the RSD of less than 0.03 (n = 5). The proposed method was applied successfully to the determination of cefetamet pivoxil in human urine and human serum.
The text was submitted by the authors in English. 相似文献
13.
Chemiluminescence assay for uric acid in human serum and urine using flow-injection with immobilized reagents technology 总被引:1,自引:0,他引:1
A novel chemiluminescence (CL) flow sensor for the determination of uric acid in human urine and serum has been developed by using controlled-reagent-release technology. The reagents involved in the chemiluminescence (CL) reaction, luminol and periodate, are immobilized on anion-exchange resin packed in a column. After injection of water, chemiluminescence generated by released luminol and periodate in alkaline media is inhibited in presence of uric acid. By measuring the decreased chemiluminescence (CL) intensity the uric acid is sensed. The decreased response is linear in the 5.0-500.0 ng mL(-1) range, with a detection limit of 1.8 ng mL(-1). The flow sensor showed remarkable operational stability and could be easily reused for over 80 h with sampling frequency of 100 h(-1). The proposed sensor was applied to the determination of uric acid in human urine and serum, and monitoring metabolic uric acid in human urine with RSD less than 3.0%. 相似文献
14.
Nakamura S Wada M Crabtree BL Reeves PM Montgomery JH Byrd HJ Harada S Kuroda N Nakashima K 《Analytical and bioanalytical chemistry》2007,387(6):1983-1990
A sensitive semi-micro column HPLC method with peroxyoxalate chemiluminescence (POCL) detection and column switching has been
developed for simultaneous determination of 3,4-methylenedioxymethamphetamine (MDMA) and related compounds, for example 3,4-methylenedioxyamphetamine,
methamphetamine, and amphetamine, in hair. After digestion of the hair with 1 mol L−1 sodium hydroxide the compounds were extracted with n-heptane and derivatized with 4-(N,N-dimethylaminosulfonyl)-7-fluoro-2,1,3-benzoxadiazole. A mixture of hydrogen peroxide and bis(2,4,5-trichloro-6-carbopentoxyphenyl)oxalate
in acetonitrile was used as post-column CL reagent. Calibration plots showed linearity was good (r = 0.999); detection limits were 0.02–0.16 ng mg−1 hair at a signal-to-noise ratio of 3. The precision of the method, as RSD (n = 5), in intra-day and inter-day assays was better than 5.0 and 6.9%, respectively. The proposed method was sufficiently
sensitive to detect low ng mg−1 levels of MDMA and related compounds in hair, and could be used for quantification of the compounds in hair samples from
patients treated in a chemical dependency unit. 相似文献
15.
Macwan JS Ionita IA Dostalek M Akhlaghi F 《Analytical and bioanalytical chemistry》2011,400(2):423-433
The aim of the proposed work was to develop and validate a simple and sensitive assay for the analysis of atorvastatin (ATV)
acid, ortho- and para-hydroxy-ATV, ATV lactone, and ortho- and para-hydroxy-ATV lactone in human plasma using liquid chromatography-tandem mass spectrometry. All six analytes and corresponding
deuterium (d5)-labeled internal standards were extracted from 50 μL of human plasma by protein precipitation. The chromatographic
separation of analytes was achieved using a Zorbax-SB Phenyl column (2.1 mm × 100 mm, 3.5 μm). The mobile phase consisted
of a gradient mixture of 0.1% v/v glacial acetic acid in 10% v/v methanol in water (solvent A) and 40% v/v methanol in acetonitrile (solvent B). All analytes including ortho- and para-hydroxy metabolites were baseline-separated within 7.0 min using a flow rate of 0.35 mL/min. Mass spectrometry detection was
carried out in positive electrospray ionization mode, with multiple-reaction monitoring scan. The calibration curves for all
analytes were linear (R
2 ≥ 0.9975, n = 3) over the concentration range of 0.05–100 ng/mL and with lower limit of quantitation of 0.05 ng/mL. Mean extraction recoveries
ranged between 88.6–111%. Intra- and inter-run mean percent accuracy were between 85–115% and percent imprecision was ≤ 15%.
Stability studies revealed that ATV acid and lactone forms were stable in plasma during bench top (6 h on ice-water slurry),
at the end of three successive freeze and thaw cycles and at −80 °C for 3 months. The method was successfully applied in a
clinical study to determine concentrations of ATV and its metabolites over 12 h post-dose in patients receiving atorvastatin. 相似文献
16.
A simple and sensitive assay was developed and validated for the simultaneous quantification of rosuvastatin acid (RST), rosuvastatin-5S-lactone (RST-LAC), and N-desmethyl rosuvastatin (DM-RST), in buffered human plasma using liquid chromatography–tandem mass spectrometry (LC-MS/MS).
All the three analytes and the corresponding deuterium-labeled (d6) internal standards were extracted from 50 μL of buffered
human plasma by protein precipitation. The analytes were chromatographically separated using a Zorbax-SB Phenyl column (2.1 mm × 100 mm,
3.5 μm). The mobile phase comprised of a gradient mixture of 0.1% v/v glacial acetic acid in 10% v/v methanol in water (solvent A) and 40% v/v methanol in acetonitrile (solvent B). The analytes were separated at baseline within 6.0 min using a flow rate of 0.35 mL/min.
Mass spectrometry detection was carried out in positive electrospray ionization mode. The calibration curves for all three
analytes were linear (R ≥ 0.9964, n = 3) over the concentration range of 0.1–100 ng/mL for RST and RST-LAC, and 0.5–100 ng/mL for DM-RST. Mean extraction recoveries
ranged within 88.0–106%. Intra- and inter-run mean percent accuracy were within 91.8–111% and percent imprecision was ≤15%.
Stability studies revealed that all the analytes were stable in matrix during bench-top (6 h on ice–water slurry), at the
end of three successive freeze and thaw cycles and at −80°C for 1 month. The method was successfully applied in a clinical
study to determine the concentrations of RST and the lactone metabolite over 12-h post-dose in patients who received a single
dose of rosuvastatin. 相似文献
17.
Clavijo CF Hoffman KL Thomas JJ Carvalho B Chu LF Drover DR Hammer GB Christians U Galinkin JL 《Analytical and bioanalytical chemistry》2011,400(3):715-728
Opioids such as morphine are the cornerstone of pain treatment. The challenge of measuring the concentrations of morphine
and its active metabolites in order to assess human pharmacokinetics and monitor therapeutic drugs in children requires assays
with high sensitivity in small blood volumes. We developed and validated a semi-automated LC-MS/MS assay for the simultaneous
quantification of morphine and its active metabolites morphine 3β-glucuronide (M3G) and morphine 6β-glucuronide (M6G) in human
plasma and in dried blood spots (DBS). Reconstitution in water (DBS only) and addition of a protein precipitation solution
containing the internal standards were the only manual steps. Morphine and its metabolites were separated on a Kinetex 2.6-μm
PFP analytical column using an acetonitrile/0.1% formic acid gradient. The analytes were detected in the positive multiple
reaction mode. In plasma, the assay had the following performance characteristics: range of reliable response of 0.25–1000 ng/mL
(r
2 > 0.99) for morphine, 1–1,000 ng/mL (r
2 > 0.99) for M3G, and 2.5–1,000 ng/mL for M6G. In DBS, the assay had a range of reliable response of 1–1,000 ng/mL (r
2 > 0.99) for morphine and M3G, and of 2.5–1,000 ng/mL for M6G. For inter-day accuracy and precision for morphine, M3G and
M6G were within 15% of the nominal values in both plasma and DBS. There was no carryover, ion suppression, or matrix interferences.
The assay fulfilled all predefined acceptance criteria, and its sensitivity using DBS samples was adequate for the measurement
of pediatric pharmacokinetic samples using a small blood of only 20–50 μL. 相似文献
18.
Beata Godlewska-ykiewicz Julita Malejko Piotr Haaburda Barbara Leniewska Anatol Kojo 《Microchemical Journal》2007,85(2):314-320
A novel flow-injection chemiluminescent (CL) method of determination of trace amounts of Pt(IV) based on its catalytic effect on the reaction of oxidation of luminol in alkaline solution is proposed. The method employs on-line separation of analyte on the column containing green algae Chlorella vulgaris immobilized on Cellex-T support. The application of biosorption process for elimination of interferences resulted in the increase in the tolerable matrix ions concentration by several orders of magnitude. The influence of dissolved organic matter on chemiluminescence of luminol was eliminated by means of a reversed phase C18 column. Under optimized conditions the suitable selectivity, good sensitivity, and low limit of detection (LOD = 0.057 ng mL− 1) of the method were obtained. The method was applied to the analysis of spiked river water samples. 相似文献
19.
A sensitive flow-injection (FI) chemiluminescence (CL) for the determination of urapidil is described in this paper. It is
based on the enhancement effect of urapidil on the CL reaction between luminol and hydrogen peroxide. The increment of CL
intensity is proportional to the concentration of urapidil in the range 0.1−10 ng/mL (R
2=0.9986), with a detection limit (3σ) of 0.03 ng/mL. The whole process, at a flow rate of 2.0 mL/min, including sampling and
washing, could be completed in 0.5 min, and the relative standard deviation (RSD) at the concentration of 0.1, 1.0, and 10.0
ng/mL was less than 3.0% (n = 5). The proposed method has been successfully applied for the determination of urapidil in pharmaceutical preparation,
human urine, and serum.
The text was submitted by the authors in English. 相似文献
20.
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