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1.
In this paper, a time-based multicommutated flow system is proposed for appropriate selection and modulation of mobile phase
composition in flow-injection (FI)/sequential-injection (SI) chromatography. The novel flow assembly involves the on-line
coupling of a short monolithic reversed-phase chromatographic column with a multisyringe flow injection set-up furnished with
a set of solenoid valves. The proposed hyphenated technique was applied to the simultaneous spectrophotometric determination
of thiamine (B1), pyridoxine (B6) and cyanocobalamin (B12) which were taken as model analytes. The separation method capitalizes on a dual isocratic elution protocol involving the
use of a single forward stroke of the multisyringe pump for initial delivery of 50 mmol L−1 ammonium acetate (pH 7.0) for 2.4 min followed by 50 mmol L−1 ammonium acetate–methanol (80:20, v/v) for 6.4 min at 0.5 mL min−1 and room temperature. Detection was performed at the maximum wavelength for each target vitamin—280 nm for B1, 325 nm for B6, and 360 nm for B12. A first-order, two-level full-factorial design was utilized to ascertain the significant variables influencing the chromatographic
separation and the magnitude of the interaction effects. The experimental design method revealed that resolution of the target
vitamins is highly dependent on the pH, percentage of organic modifier, and their second-order interaction. The multisyringe
flow-injection-based monolithic column separation method, which should be viewed as an expeditious and cost-effective alternative
to the high-performance liquid chromatography counterpart, was applied to the separation and determination of B1, B6, and B12 in different pharmaceutical dosage forms in less than 9 min. Statistical comparison of the results from the proposed procedure
with those from the HPLC method endorsed by the US Pharmacopeia revealed there were no significant differences at the 95 %
confidence level. 相似文献
2.
Marcela Z. Arend Simone G. Cardoso Felipe K. Hurtado Aline Ravanello Fibele A. Lanzanova Clarice M. B. Rolim 《Chromatographia》2009,69(Z2):195-199
A simple stability-indicating reversed-phase liquid chromatographic method with diode-array detection was developed and validated
for the quantitative determination of ebastine in tablets and syrup. The LC method was carried out on a C18 column with acetonitrile:phosphoric acid 0.1% pH 3.0 (55:45, v/v) as mobile phase, at a flow rate of 1.2 mL min−1. Ultraviolet detection of ebastine was at 254 nm. A linear response (r = 0.9999) was observed in the range of 10–80 μg mL−1. The RSD values for intra- and inter-day precision studies showed good results (RSD < 2%) and accuracy was greater than 98%.
Validation parameters such as specificity and robustness were also determined. The method was found to be stability-indicating
and can be applied to quantitative determination of ebastine in tablets and syrup. 相似文献
3.
Huang KJ Zhang M Xie WZ Zhang HS Feng YQ Wang H 《Analytical and bioanalytical chemistry》2007,388(4):939-946
A simple, sensitive, selective, and low-cost method is proposed for rapidly determining nitric oxide (NO) in some rat tissues.
Polymer monolith microextraction (PMME) using a poly(methacrylic acid–ethylene glycol dimethacrylate) (MAA-EGDMA) monolithic
column was combined with derivatization of NO using 1,3,5,7-tetramethyl-8-(3′,4′-diaminophenyl)-difluoroboradiaza-s-indacene (TMDABODIPY), and this was used to analyze the derivatives of NO by high-performance liquid chromatography (HPLC)
with fluorescence detection at λ
ex/λ
em = 498/507 nm. The baseline separation of TMDABODIPY and its NO derivative is performed under simple conditions in which a
C18 column is used and eluted with 50 mmol L−1 ethanolamine and methanol. The conditions for the extraction of NO derivatives were optimized. The limit of detection of
NO was 2 × 10−12 mol L−1 (S/N = 3). The linearity range of the method was 9 × 10−11−4.5 × 10−8 mol L−1. The interday and intraday relative standard deviations were less than 5%. The proposed method was successfully applied to
the determination of NO levels in some rat tissue samples including heart, kidney, and liver with recoveries varying from
87.1 to 95.2%. 相似文献
4.
Summary A new, rapid, and precise liquid chromatographic method has been developed for simultaneous identification and quantification
of amphetamine,N-methyl-3,4-methylenedioxymetamphetamine,N-ethyl-3,4-methylenedioxymetamphetamine, andN-methyl-1-(3,4-methyl-enedioxyphenyl)-2-butanamine in the presence of other constituents. The compounds were separated on
a monolithic column with a gradient prepared from acetonitrile and 20mm monobasic potassium buffer at a flow rate of 1.5 mL min−1. Quantitation was performed with metoclopramide as internal standard. Use of different flow rates was investigated and enabled
reduction of the separation time from 11 to 3.5 min for seven substances. The method was then applied to ten seized tablets
to identify and quantify their active ingredients. 相似文献
5.
This paper describes the development of a new multisyringe flow injection analysis set-up that enables the complete automation
of the dispersive liquid–liquid microextraction (DLLME) technique using solvents lighter than water. Its hyphenation with
a liquid chromatographic separation is implemented using a single multisyringe pump obtaining a compact, simple, easy to operate,
and fast instrument. DLLME is carried out with a throughput of 42 h−1 and DLLME for the extraction of benzo(a)pyrene and its subsequent chromatographic determination can be carried out with an
analysis throughput of 7 h−1. 相似文献
6.
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
7.
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
8.
In the present study, a rapid and sensitive LC-ESI-MS/MS method for quantification of (S)-fluoxetine as a native marker in mass spectrometry (MS) binding assays addressing the human serotonin transporter (hSERT)
was developed and validated. The concept of MS binding assays based on mass spectrometric quantification of a nonlabeled marker
recently introduced by us represents a promising alternative to conventional radioligand binding without the drawbacks inherently
connected with radioisotope labeling. For high-performance liquid chromatography (HPLC), a 20 × 2-mm RP-18 column with a mobile
phase composed of acetonitrile and ammonium bicarbonate buffer (5 mmol L−1, pH 9.5) at a ratio of 80:20 (v/v) and a flow rate of 800 μL min−1 in an isocratic mode were used, resulting in a chromatographic cycle time of 60 s. Employing [2H5]fluoxetine as internal standard enabled ESI-MS/MS quantification of (S)-fluoxetine between 3 nmol L−1 and 50 pmol L−1 (LLOQ) in matrix obtained from binding experiments without the need of any sample preparation. Validation of the method showed
that linearity, intra-, and inter-batch accuracy as well as precision meet the requirements of the FDA guidance for bioanalytical
method validation. Considering sensitivity and speed, the established method is clearly superior to those published for biological
matrices so far. Furthermore, the method was transferred to other RP-18 columns of different lengths and respective validation
experiments demonstrated its versatility and chromatographic robustness. Finally, the newly developed method was successfully
applied to MS binding assays for hSERT. The affinity determined for (S)-fluoxetine in saturation experiments was in good agreement with literature data obtained in respective radioligand binding
assays. 相似文献
9.
Marcelo Donadel Malesuik Simone Gonçalves Cardoso Martin Steppe 《Chromatographia》2008,67(1-2):131-136
A reversed-phase liquid chromatographic (LC) method was developed for the assay of nitazoxanide (NTZ) in solid dosage formulations.
An isocratic LC separation was performed on a Phenomenex Synergi Fusion C18 column (250 mm × 4.6 mm, i.d., 4 μm particle size) using a mobile phase of 0.1% o-phosphoric acid solution, pH 6.0: acetonitrile (45:55, v/v) at a flow rate of 1.0 mL min−1. Detection was achieved with a photodiode array detector at 240 nm. The detector response for NTZ was linear over the concentration
range from 2 to 100 μg mL−1 (r = 0.9999). The specificity and stability-indicating capability of the method were proved using stress conditions. The RSD
values for intra-day precision were less than 1.0% for tablets and powder for oral suspension. The RSD values for inter-day
precision were 0.6 and 0.7% for tablets and powder for oral suspension. The accuracy was 100.4% (RSD = 1.8%) for tablets and
100.9% (RSD = 0.3%) for powder for oral suspension. The limits of quantitation and detection were 0.4 and 0.1 μg mL−1. There was no interference of the excipients on the determination of the active pharmaceutical ingredient. The proposed method
was precise, accurate, specific, and sensitive. It can be applied to the quantitative determination of drug in tablets and
powder for oral suspension. 相似文献
10.
León Z Balaguer A Chisvert A Salvador A Herráez M Díez O 《Analytical and bioanalytical chemistry》2008,391(3):859-866
An analytical method based on ion-interaction chromatography with UV detection for simultaneous in-vitro estimation of the
percutaneous absorption of the most used water-soluble UV filters in sunscreen cosmetics is proposed. These UV filters were
phenylbenzimidazole sulfonic acid, disodium phenyl dibenzimidazole tetrasulfonate, benzophenone-4, and terephthalylidene dicamphor
sulfonic acid. The methodology is based on applying the sunscreen containing the target UV filters to human epidermis in a
diffusion cell. Analytes are determined in the receptor solution. To ensure skin integrity, screening of the cells was carried
out by analytical determination of a marker. Analytical variables such as percentage ethanol, concentration of ion-pairing
agent, pH of the mobile phase, and temperature were studied in order to achieve high resolution of the chromatographic peaks
in the lowest possible time of analysis. The conditions selected consisted of a mobile phase composed of 35:65 (v/v) ethanol–ammonium acetate buffer solution (pH 4, containing 50 mmol L−1 tetra-n-butylammonium bromide). The chromatographic determination was carried out with the analytical column at 50 °C. UV detection
was carried out at the maximum absorption wavelength for each analyte. The limit of detection (3s
y/x
/b) ranged from 16 to 65 ng mL−1, depending on the analyte. 相似文献
11.
Zhang ZX Gao PF Guo XF Wang H Zhang HS 《Analytical and bioanalytical chemistry》2011,401(6):1905-1914
1,3,5,7-Tetramethyl-8-(N-hydroxysuccinimidyl butyric ester)difluoroboradiaza-s-indacene (TMBB-Su), a new BODIPY-based fluorescent probe, was designed and synthesized for the labeling of amino compounds.
It was used as a pre-column derivatizing reagent for determination of amino acid neurotransmitters by high-performance liquid
chromatography (HPLC). The fluorescence quantum yield in acetonitrile increased from 0.84 to 0.95 when it reacted with amino
acid neurotransmitters. Derivatization of TMBB-Su with seven amino acid neurotransmitters was completed within 30 min at 25 °C
in 24.0 mmol L−1 pH 7.8 boric acid buffer. The separation was performed on a C18 column with methanol–water–buffer 55:35:10 (v/v) as mobile phase (buffer: 0.10 mol L−1 H3Cit–0.10 mol L−1 NaOH). Interference from the other concomitant amino acids was eliminated successfully by means of pH gradient elution. With
fluorescence detection at 494 and 504 nm for excitation and emission, respectively, the limits of detection (signal-to-noise
ratio = 3) were from 2.1 to 12.0 nmol L−1. The proposed method has been used to determine amino acid neurotransmitters in the cerebral cortex of mice with cerebral
ischemia at the convalescence stage with satisfactory recoveries varying from 94.9 to 105.2%. 相似文献
12.
Letícia Flores da Silva Martins Pedro Eduardo Froehlich Ana Maria Bergold 《Chromatographia》2009,69(Z2):109-113
A sensitive and rapid liquid chromatographic method was successfully developed and validated for the determination of sibutramine
hydrochloride in bulk and capsules. Sibutramine in the presence of its degradation products was analyzed using UV detection
at 225 nm. Chromatography was performed on a reversed-phase C8 (150 × 4.0 mm I.D., 5 μm) analytical column under isocratic conditions. The mobile phase was composed of acetonitrile:water
(aqueous phase containing 0.3% triethylamine and pH adjusted to 7.0) (75:25, v/v) at a flow-rate of 1.1 mL min−1. No chromatographic interference was found during the analysis. Light was the stress condition which most contributed to
sibutramine degradation. The method showed a linear response (r > 0.999) from 30 to 90 μg mL−1. The mean recovery for capsules was 101.2%. Inter-day assays showed relative standard deviations of 0.42 and 1.62% for bulk
and capsules, respectively. The developed method is able to separate sibutramine from its major degradation products and it
may be used in the quality control of this active pharmaceutical ingredient in both bulk and capsules. 相似文献
13.
A simple, rapid, and precise reversed-phase high-performance liquid chromatographic method has been developed for simultaneous determination of losartan potassium, ramipril, and hydrochlorothiazide. The three drugs were separated on a 150 mm × 4.6 mm i.d., 5 μm particle, Cosmosil C18 column. The mobile phase was 0.025 m sodium perchlorate–acetonitrile, 62:38 (v/v), containing 0.1% heptanesulphonic acid, pH adjusted to 2.85 with orthophosphoric acid, at a flow rate of 1.0 mL min−1. UV detection was performed at 215 nm. The method was validated for linearity, accuracy, precision, and limit of quantitation. Linearity, accuracy, and precision were acceptable in the ranges 35–65 μg mL−1 for losartan, 1.75–3.25 μg mL−1 for ramipril, and 8.75–16.25 μg mL−1 for hydrochlorothiazide. 相似文献
14.
Shao-Wen Zhang Jun Xing Ling-Shuang Cai Cai-Ying Wu 《Analytical and bioanalytical chemistry》2009,395(2):479-487
Urinary 8-hydroxy-2′-deoxyguanosine (8-OHdG) has been widely used as a biomarker of oxidative DNA damage. Measurements of
8-OHdG in urinary samples are challenging owing to the low level of 8-OHdG and the complex matrix. In this study, a novel
molecularly imprinted polymer (MIP) monolithic column was synthesized with guanosine as a dummy template which was used as
the medium for in-tube solid-phase microextraction (SPME). In-tube SPME coupled with HPLC/UV detection for extraction and
determination of urinary 8-OHdG was developed. The synthesized MIP monolithic column exhibited high extraction efficiency
owing to its greater phase ratio with convective mass transfer and inherent selectivity. The enrichment factor for 8-OHdG
was found to be 76 and the limits of detection and quantification of the method for urinary samples were 3.2 nmol/L (signal-to-noise
ratio 3) and 11 nmol/L (signal-to-noise ratio 10), respectively. The MIP’s selectivity also made the sample preparation procedure and chromatographic separation much easier. The linear range of the
proposed method was from 0.010 to 5.30 μmol/L (r = 0.9997), with a relative standard deviation of 1.1–6.8%, and the recovery for spiked urine samples was 84 ± 3%. The newly
developed method was successfully applied to determine urinary samples of healthy volunteers, coking plant workers, and cancer
patients. The 8-OHdG level in cancer patients was significantly higher than that in healthy people. 相似文献
15.
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
16.
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
17.
Jing Bai Jean Chrysostome Ndamanisha Lin Liu Li Yang Liping Guo 《Journal of Solid State Electrochemistry》2010,14(12):2251-2256
The potential application of ordered mesoporous carbon (OMC)-modified glassy carbon electrode (OMC/GCE) in electrochemistry
as a novel electrode material was investigated. X-ray diffraction, transmission electron micrographs, and cyclic voltammetry
were used to characterize the structure and electrochemical behaviors of this material. Compared to GC electrode, the peak
currents of potassium ferricyanide (K3[Fe(CN)6]) increase and the peak potential separation (ΔE
p) decreases at the OMC/GC electrode. These phenomena suggest that OMC-modified GC electrode possesses larger electrode area
and faster electron transfer rate, as compared with bare GC electrode. Furthermore, riboflavin was detected using OMC/GC electrode
in aqueous solutions. The results showed that, under an optimum condition (pH 7.0), the OMC/GC electrode exhibited excellent
response performance to riboflavin in the concentration range of 4.0 × 10−7 to 1.0 × 10−6 M with a high sensitivity of 769 μA mM−1. The detection limit was down to around 2 × 10−8 M. With good stability and reproducibility, the present OMC/GC electrode was applied in the determination of vitamin B2 content in vitamin tablets, and satisfactory results were obtained. 相似文献
18.
A. Mancha de Llanos M. M. De Zan M. J. Culzoni A. Espinosa-Mansilla F. Cañada-Cañada A. Muñoz de la Peña H. C. Goicoechea 《Analytical and bioanalytical chemistry》2011,399(6):2123-2135
A liquid chromatographic method has been developed, in combination with the multivariate curve resolution-alternating least
squares algorithm (MCR-ALS), for the simultaneous determination of marker pteridines in urine samples. A central composite
design has been applied to optimize the factors influencing the separation (buffer concentration, buffer pH, flow rate, oven
temperature, mobile-phase composition). A set of 15 calibration samples were randomly prepared, in a concentration range of
0.5–10.5 ng mL−1 for neopterin, biopterin, and pterin; 4.0–8.0 ng mL−1 for xanthopterin; and 0.5–4.5 ng mL−1 for isoxanthopterin. The validation was carried out with fortified urine samples from healthy adults. The optimized conditions
were a mobile-phase composition of 10 mM citric buffer at pH 5.44 and acetonitrile (94.5/5.5, v/v), a flow rate of 1.0 mL min−1, and an oven temperature of 25 °C. The detection system consisted of a fast-scanning spectrofluorimeter, which allows obtaining
of second-order data matrices containing the fluorescence intensity as a function of retention time and emission wavelength.
In this work, MCR-ALS was used to cope with coeluting interferences, on account of the second-order advantage inherent to
this algorithm which, in addition, is able to handle data sets deviating from trilinearity, like the high-performance liquid
chromatography data analyzed in the present report. The developed approach enabled us to determine five pteridines, some of
them with overlapped profiles, reducing the experimental time and reagent consumption. Ratio values for pteridines/creatinine
in urine, for infected children with different pathologies, are reported in this work. 相似文献
19.
Combined use of carbon nanotubes and ionic liquid to improve the determination of antidepressants in urine samples by liquid chromatography 总被引:1,自引:0,他引:1
Cruz-Vera M Lucena R Cárdenas S Valcárcel M 《Analytical and bioanalytical chemistry》2008,391(4):1139-1145
Antidepressants are widely used for the treatment of psychiatric disorders and therefore their monitoring in biological fluids
is quite important taking into account that they can produce dangerous biochemical imbalances in toxic doses. A method for
the determination of antidepressants in urine samples is presented using solid-phase extraction (SPE) and high-performance
liquid chromatography (HPLC) with ultraviolet (UV) detection. Home-made cartridges containing 30 mg multiwall carbon nanotubes
are employed for isolation of the analytes from the sample, allowing also the preconcentration of the analytes prior to the
HPLC analysis. Chromatographic separation was achieved in a reversed-phase C8 column using the ionic liquid 1-butyl-3-methylimidazolium trifluoromethanesulfonate as silanol activity suppressor, which
enhances peak symmetry and chromatographic resolution. Limits of detection were 12.3 ng mL−1 for trazodone and 90.1 ng mL−1 for fluoxetine. The repeatability of the proposed method expressed as RSD (n = 11) varied between 3.4% (fluoxetine) and 5.0% (desipramine and mianserine). Thus, the method is suitable for the therapeutic
monitoring of antidepressants in urine samples. 相似文献
20.
A. Önal 《Chromatographia》2006,64(7-8):459-461
A reversed-phase high-performance liquid chromatographic (HPLC) method with UV detection was developed and validated for the determination of ropinirole (ROP) in tablets. The assay utilized UV detection at 250 nm and a Luna CN column (250 × 4.6 mm I.D, 5 μm). The mobile phases were comprised of acetonitrile: 10 mM nitric acid (pH 3.0) (75:25, v/v). Validation experiments were performed to demonstrate linearity, accuracy, precision, limit of quantitation (LOQ), limit of detection (LOD), and robustness. The method was linear over the concentration range of 0.5–10.0 μg mL−1. The method showed good recoveries (99.75–100.20%) and the relative standard deviations of intra and inter-day assays were 0.38–1.69 and 0.45–1.95%, respectively. The method can be used for quality control assay of ropinirole. 相似文献