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1.
A simple reversed-phase high-performance liquid chromatographic (HPLC) method has been developed for the simultaneous determination
of the antiepileptic drugs (AEDs) zonisamide (ZNS), primidone (PRI), lamotrigine (LTG), phenobarbital (PB), phenytoin (PHT),
oxcarbazepine (OXC), and carbamazepine (CBZ) and two of their active metabolites, monohydroxycarbamazepine (MHD) and carbamazepine
10,11-epoxide (CBZE) in human plasma. Plasma (100 μL) was pretreated by deproteinization with 300 μL methanol containing 20 μg mL−1 propranolol hydrochloride as internal standard. HPLC was performed on a C8 column (4.6 mm × 250 mm; particle size 5 μm) with methanol–acetonitrile–0.1% trifluoroacetic acid, 235:120:645 (v/v), as mobile phase at a flow rate of 1.5 mL min−1. ZNS, OXC, and CBZ were monitored by UV detection at 235 nm, and PRI, LTG, MHD, PB, PHT, and CBZE by UV detection at 215 nm.
Relationships between response and concentration were linear over the concentration ranges 1–80 μg mL−1 for ZNS, 5–50 μg mL−1 for PRI, 1–25 μg mL−1 for LTG, 1–50 μg mL−1 for MHD, 5–100 μg mL−1 for PB, 1–10 μg mL−1 for CBZE, 0.5–25 μg mL−1 for OXC, 1–50 μg mL−1 for PHT, and 1–25 μg mL−1 for CBZ. Intra-day and inter-day reproducibility were adequate (coefficients of variation were ≤11.6%) and absolute recovery
ranged from 95.2 ± 6.13 to 107.7 ± 7.76% for all the analytes; for the IS recovery was 98.69 ± 1.12%. The method was proved
to be accurate, reproducible, convenient, and suitable for therapeutic monitoring of the nine analytes. 相似文献
2.
Lei Zhang Liang Xu Xiao-Jie Tan Qiong-Feng Liao Wei Guo Xiao-Hui Chen Kai-Shun Bi 《Chromatographia》2007,66(1-2):115-120
A sensitive and reliable ion-paired high-performance liquid chromatographic method has been established for the simultaneous
quantification of six major active ingredients, namely baicalin, baicalein, wogonin, oxysophocarpine, oxymatrine and matrine
in the Chinese herbal preparation, Sanwu-Huangqin-Tang. HPLC analyses were performed on a Phenomenex luna C18 column with mobile phase of methanol–acetonitrile–aqueous phosphoric acid at a flow rate of 0.9 mL min−1. The complete separation was achieved within 35 min for the six target constituents. A good linear regression relationship
between peak-areas and concentrations was obtained over the range of 12.10–242.0 μg*mL−1 for baicalin, 5.05–101.0 μg*mL−1 for baicalein, 0.95–19.0 μg*mL−1 for wogonin, 2.75–55.0 μg*mL−1 for oxysophocarpin, 2.75–55.0 μg*mL−1 for oxymatrine and 4.90–98.0 μg*mL−1 for matrine, respectively. The repeatability was evaluated by intra- and inter-day assays with relative standard deviation
(RSD) being less than 5.1%. The recoveries, measured at three concentration levels, varied from 93.8 to 102.1%. The assay
was successfully applied for determination of six bioactive compounds in Sanwu-Huangqin-Tang. The interaction of chemical
constituents was observed when the herbs were used in compatibility. The results indicated that the developed assay method
was rapid, accurate and could be readily utilized as a quality control method for Sanwu-Huangqin-Tang. 相似文献
3.
Cantú MD Toso DR Lacerda CA Lanças FM Carrilho E Queiroz ME 《Analytical and bioanalytical chemistry》2006,386(2):256-263
Simple, sensitive, and reproducible off-line solid-phase microextraction and liquid chromatography (SPME/LC) methods are described
for the determination of seven anticonvulsants and tricyclic antidepressants in human plasma. Factorial design and simplex
methodology were applied in the optimization of the SPME procedure for tricyclic antidepressants analyses. Important factors
in the SPME efficiency are discussed, such as the fiber coatings (both lab-made and commercial), extraction time, pH, ionic
strength, influence of plasma proteins, and desorption conditions. The development of the lab-made fiber coatings, namely,
octadecylsilane, aminosilane, and polyurethane, are further described and applied to anticonvulsants analyses. The investigated
plasmatic range for the evaluated anticonvulsants, using CW-TPR fiber, were the following: phenylethylmalonamide (3.00–40.0 μg
mL−1), phenobarbital (5.00–40.0 μg mL−1), primidone (3.00–40.0 μg mL−1), carbamazepine and carbamazepine-epoxide (2.00–24.0 μg mL−1), phenytoin (2.00–40.0 μg mL−1), and lamotrigine (0.50–12.0 μg mL−1). The antidepressants’ linear plasmatic concentration ranged from 75.0 to 500 ng mL−1 for imipramine, amitriptyline, and desipramine, and from 50.0 to 500 ng mL−1 for nortriptyline, being in all cases, the limit of quantification represented by the lowest value. The precision (interassays)
for all investigated drugs in plasma sample spiked with different concentrations of each analyte and submitted to the described
procedures were lower than 15%. The off-line SPME/LC methodologies developed allow anticonvulsants and antidepressants analyses
from therapeutic to toxic levels for therapeutic drug monitoring. 相似文献
4.
M. A. Campanero A. M. Zamarreño M. Simón M. C. Dios J. R. Azanza 《Chromatographia》1997,46(7-8):374-380
Summary A simple and rapid liquid chromatographic method has been developed for the determination of therapeutic levels of piperacillin
(I) and ceftazidime (II) in human plasma. Plasma and p-propionamidophenol (internal standard) were precipitated with methanol
(I) or 20% trichloroacetic acid (II). The supernatant was analysed on a 5 μm Spherisorb ODS C18 column with acetonitrile-0.05 M phosphate buffer pH 3.8 as mobile phase and ultraviolet detection at 254 nm. The calibration
graph was linear from 10 to 250 μg mL−1, for (I), and from 5 to 200 μg mL−1 for (II). Intra and inter-day CV did no exceed 2.29% for (I), and were 10.76–11.13%–2.00–5.62 for (II) at concentrations
of 10 μg mL−1 and 250 μg mL−1. 相似文献
5.
A high-performance liquid chromatography–UV method for determining DCJW concentration in rat plasma was developed. The method
described was applied to a pharmacokinetics study of intramuscular injection in rats. The plasma samples were deproteinized
with acetonitrile in a one-step extraction. The HPLC assay was carried out using a VP-ODS column and the mobile phase consisting
of acetonitrile–water (80:20, v/v) was used at a flow rate of 1.0 mL min−1 for the effective eluting DCJW. The detection of the analyte peak area was achieved by setting a UV detector at 314 nm with
no interfering plasma peak. The method was fully validated with the following validation parameters: linearity range 0.06–10 μg mL−1 (r > 0.999); absolute recoveries of DCJW were 97.44–103.46% from rat plasma; limit of quantification, 0.06 μg mL−1 and limit of detection, 0.02 μg mL−1. The method was further used to determine the concentration–time profiles of DCJW in the rat plasma following intramuscular
injection of DCJW solution at a dose of 1.2 mg kg−1. Maximum plasma concentration (C
max) and area under the plasma concentration–time curve (AUC) for DCJW were 140.20 ng mL−1 and 2405.28 ng h mL−1. 相似文献
6.
Tetracycline antibiotics (TCs) such as doxycycline (DOTC), chlortetracycline (CTC), oxytetracycline (OTC), and tetracycline
(TC) react with Cu(II) in pH 3.5 BR buffer medium to form 1:1 cationic chelates, which further react with titan yellow to
form 2:1 ion association complexes. These result in great enhancement of resonance Rayleigh scattering (RRS) and the appearance
of new RRS spectra. The ion association complexes of DOTC, CTC, OTC, and TC have similar spectral characteristics and their
maximum RRS wavelengths are all located at 464 nm. The quantitative determination ranges and the detection limits (3σ) of the four TCs are 0.037–4.8 μg mL−1 and 11.2 ng mL−1 for DOTC, 0.041–5.2 μg mL−1 and 12.4 ng mL−1 for CTC, 0.050–4.8 μg mL−1 and 15.1 ng mL−1 for TC, and 0.088–5.0 μg mL−1 and 26.3 ng mL−1 for OTC, respectively. The optimum reaction conditions, the effects of foreign substances, the structure of ternary complexes,
and the reaction mechanism are discussed. A sensitive, rapid, and simple RRS method for the determination of DOTC has been
developed. 相似文献
7.
A new method was developed for the simultaneous determination of lidocaine, proline and lomefloxacin in human urine by capillary
electrophoresis-electrochemiluminescence detection with Ru(bpy)3
2+. Conditions of the separation and detection were investigated and optimized. It was proved that 20 mM phosphate buffer at
pH 6.7 could achieve the most favorable resolution, and the high sensitivity of detection was obtained by using the detection
potential at 1.15 V and 5 mM Ru(bpy)3
2+–60 mM phosphate buffer at pH 7.6 in the detection reservoir. The detection limits were 0.02 μg mL−1 for lidocaine, 0.03 μg mL−1 for proline and 0.06 μg mL−1 for lomefloxacin. Relative standard deviations of the ECL intensity and the migration time were 3.5 and 1.1% for 6 μg mL−1 lidocaine, 3.2 and 1.0% for 6 μg mL−1 proline and 3.7 and 1.2% for 6 μg mL−1 lomefloxacin, respectively. A baseline separation for lidocaine, proline and lomefloxacin was achieved within 360 s. The
developed method was successfully applied to determine the amounts of lidocaine, proline and lomefloxacin in human urine.
The recovery and RSD were in the range of 93.3–97.2 and 3.8–4.9%, respectively. 相似文献
8.
A novel kinetic spectrofluorimetric method for the determination of uric acid based on the activation effect of uric acid
on the Cu(II) ion catalyzed oxidation of pyronine Y by hydrogen peroxide was developed. The influence of different buffer
solutions was tested and the Britton-Robinson buffer solution with pH 2.2 was found to be the optimum. The detection limit
and the linear range for uric acid are 0.09 μg mL−1 and 0.3–3.0 μg mL−1, respectively. The RSD for eleven determinations of 1.6 μg mL−1 uric acid was 1.6 %. Satisfactory results were obtained when using this method of uric acid determination in human urine. 相似文献
9.
Graziele P. Ramos Paula M. B. Dias Cláudia B. Morais Pedro E. Fröehlich Miguel Dall’Agnol José A. S. Zuanazzi 《Chromatographia》2008,67(1-2):125-129
Red clover (Trifolium pratense L.) is an important forage plant that contains the isoflavones daidzein, genistein, formononetin, and biochanin A. These
compounds have been studied lately due to their human health benefits. The aim of this study was to develop and validate an
HPLC method with simplified sample preparation to quantify daidzein, genistein, formononetin and biochanin A simultaneously
in red clover leaves. The validation showed that the method is specific, accurate, precise and robust, not to mention that
the sample preparation is easier and faster than those described earlier. The response was linear over a range of 0.01–0.2 μg mL−1 for daidzein, 0.05–0.5 μg mL−1 for genistein, 4–40 μg mL−1 for formononetin and 2–20 μg mL−1 for biochanin A. The range of recoveries was 85.6–101.0%. The RSD for intra- and inter-day precision were <2.54 and <7.22%,
respectively. Five populations of red clover, from the National Plant Germplasm System-USDA were analyzed and the content
of daidzein, genistein, formononetin and biochanin A ranged from 7.87–91.31, 51.60–131.30, 6568.33–23461.82, to 2499.55–10337.33 μg g−1 of dried material, respectively. 相似文献
10.
Protein can greatly enhance the fluorescence of curcumin (CU) in the presence of sodium dodecyl benzene sulfonate (SDBS).
Experiments indicate that under the optimum conditions, the enhanced intensity of fluorescence is proportional to the concentration
of proteins in the range of 0.0050–20.0 μg mL−1 for bovine serum albumin (BSA), 0.080–20.0 μg mL−1 for human serum albumin (HSA), and 0.040–28.0 μg mL−1 for egg albumin (EA). Their detection limits (S/N=3) are 1.4 ng mL−1, 20 ng mL−1, and 16 ng mL−1, respectively. The method has been satisfactorily used for the determination of proteins in actual samples. In comparison
with most of fluorimetric methods, this method is quick and simple, has high sensitivity and good stability. The interaction
mechanism is also studied. 相似文献
11.
Summary A simple and rugged SPE method for the determination of tetracycline (TC), minocycline (MC) and demeclocycline (DCC) in porcine
serum by high performance liquid chromatography (HPLC) was developed. The spiked serum sample was pretreated with 2% phosphoric
acid followed by a simple and rugged solid-phase extraction procedure using the OasisTM HLB extraction cartridges. High and reproducible recoveries were obtained even though the cartridges were run dry. The extracted
sample analytes were injected onto a Waters SymmetryShieldTM RP8 column. The mobile phase was a simple volatile solution containing 0.1% TFA, 2% methanol and 7% acetonitrile in Water. The
antibiotics were detected at 350 nm. The calibration curves were linear from 2.0 to 25.0 μg mL−1 of TC and MC with DCC as the internal standard at a concentration of 25.0 μg mL−1. For six replicate analyses, the average recoveries of TC and MC from porcine serum sample fortified at the level of 2.5
μg mL−1 were 96.1% with 1.3% RSD and 101% with 0.54% RSD; at level of 0.5 μg mL−1 the average recoveries were 88% with 1.6% RSD and 97.8% with 1.4% RSD. 相似文献
12.
A reverse phase HPLC method was developed and validated for the simultaneous determination of 2-hydroxy-4-methoxybenzaldehyde
and 2-hydroxy-4-methoxybenzoic acid in the root extracts of Hemidesmus indicus. A comprehensive validation of the method including sensitivity, linearity, reproducibility, accuracy, limit of detection
(LOD) and limit of quantification (LOQ) was conducted using the optimized chromatographic conditions. The method was found
to be linear (r > 0.998) in the range of 5–350 μg mL−1 for 2-hydroxy-4-methoxybenzaldehyde and for 2-hydroxy-4-methoxybenzoic acid (r > 0.999) in the range 10–300 μg mL−1. The method was found to be precise with inter-day precision values (% RSD) in the ranges of 0.61–1.76% for 2-hydroxy-4-methoxybenzaldehyde
and 1.3–2.8% for 2-hydroxy-4-ethoxybenzoic acid while intra-day precisions (% RSD) of two analytes were in the range of 0.41–1.07
and 0.95–2.5%. The limits of detection (LODs) for 2-hydroxy-4-methoxybenzaldehyde and 2-hydroxy-4-methoxybenzoic acid were
0.84 and 2.34 μg mL−1. The described method was fast, sensitive and reproducible, and thus well suited for routine analysis of these two compounds
from root extracts of H. indicus and other plants. 相似文献
13.
A sensitive analytical method was established for the determination of Th and U in activated concrete samples. The method
combines an anion-exchange separation step with an ICP-MS determination technique. In the ICP-MS measurement, a few μg mL–1 of Al and Ca, a few ng mL–1 of Mn, La, Ce, Nd and Pb and pg mL–1 amounts of Li, Zr, Nb and Ba coexisting in the anion-exchange fraction of Th and U did not interfere. No adverse interference
effects were observed in real sample analyses. The obtained detection limits (3σ, n = 10) of Th and U were 2.3 and 1.8 pg mL–1, respectively. The analytical precisions for ca. 5 μg g–1 Th and ca. 1 μg g–1 U in real activated concrete samples were equally less than 7% RSD. The accuracies obtained by the analysis of GSJ rock standard
samples were –18.1 to 0.4% for the Th determination and –14.0 to –5.7% for the U determination. The method uses the conventional
absolute calibration curve. The internal standard calibration is unnecessary.
Received: 14 March 1999 / Revised: 13 July 1999 / Accepted: 15 July 1999 相似文献
14.
Summary A reversed-phase ion-pair chromatographic (RPIPC) method withN,N,N′, N′-ethylenediaminetetrakis(methylenephosphonic acid) (EDTMP) as coordinating agent has been developed for simultaneous separation
and detection of Cu(II), Fe(III), and Pb(II) ions. Response is linearly dependent on amount of sample over the range 9.52–50.8
μg mL−1 for Cu(II), 8.31–41.8 μg mL−1 for Fe(III), and 37.3–51.8 μg mL−1 for Pb(II). The method has been applied successfully to an artificial mixed-ore sample. 相似文献
15.
A micelle eletrokinetic capillary chromatography (MEKC) method was used to determine Danshensu in rabbit blood plasma and
tissues (liver, lung, kidney, brain, heart and spleen). The separation was achieved with a buffer consisting of 30 mmol L−1 borax and 50 mmol L−1 SDS (pH 9.0), and with an applied voltage of 7.0 kV. Validation of the method showed good sensitivity, reproducibility and
precision. The calibration curve for Danshensu was linear over the concentration range of 0.4–400 μg mL−1. The limit of detection (LOD) was 0.08 μg mL−1 (S/N = 3). The validated method has been successfully applied for the pharmacokinetic and the tissue distribution studies
of Danshensu after intragastric administration of the aqueous extract from traditional Chinese medicine Danshen. 相似文献
16.
Determination of phenazopyridine in human plasma by high performance liquid chromatography 总被引:1,自引:0,他引:1
Summary A simple, low-cost, sensitive and selective HPLC method was developed for the determination of phenazopyridine in human plasma.
The method employs UV detection of phenazopyridine and of the internal Standard at 2 different wavelengths. Calibration curves
were linear over a large dynamic range, i.e., within 0.05–10.0 μg mL−1 with limit of quantification of 0.05 μg mL−1, and a limit of detection of 0.01 μg mL−1. 相似文献
17.
A. Ruiz Medina M. L. Fernández de Córdova A. Molina Díaz 《Analytical and bioanalytical chemistry》1999,365(7):619-624
A new, sensitive and very simple spectrofluorimetric biparameter sensor is described for the determination of salicylamide
and/or salicylic acid in pharmaceutical preparations. The method integrates the transitory retention and fluorescence detection
of both compounds on Sephadex QAE A-25 resin packed into a conventional flow-through cell. A monochannel manifold with two
alternative carriers is used. At pH 2.0 (first carrier) salicylic acid is selectively retained on the solid support and after
developing the analytical signal it is desorbed. At pH 11.0 (second carrier) both salicylic acid and salicylamide are simultaneously
and transitorily retained on the solid, the analytical signal now corresponding to both analytes. The monochromators were
tuned at 260 (excitation) and 415 (emission) nm, respectively. The calibration graph for salicylamide is linear over the range
0.01 to 0.32 μg mL–1 and for salicylic acid from 0.04 to 1.0 μg mL–1 in the presence of each other. The relative standard deviation and the sampling frequency for the determination of salicylamide
(0.20 μg mL–1) and salicylic acid (0.50 μg mL–1) were 1.1% and 35 h–1, and 0.9% and 45 h–1, respectively. Good results on application to individual determination or mixture resolution in pharmaceutical samples testify
to the usefulness of the proposed sensor.
Received: 20 April 1999 / Revised: 7 June 1999 / Accepted: 12 June 1999 相似文献
18.
Michael Winklmair Andreas J. Schuetz M. G. Weller Reinhard Niessner 《Fresenius' Journal of Analytical Chemistry》1999,363(7):619-624
A new, sensitive and very simple spectrofluorimetric biparameter sensor is described for the determination of salicylamide
and/or salicylic acid in pharmaceutical preparations. The method integrates the transitory retention and fluorescence detection
of both compounds on Sephadex QAE A-25 resin packed into a conventional flow-through cell. A monochannel manifold with two
alternative carriers is used. At pH 2.0 (first carrier) salicylic acid is selectively retained on the solid support and after
developing the analytical signal it is desorbed. At pH 11.0 (second carrier) both salicylic acid and salicylamide are simultaneously
and transitorily retained on the solid, the analytical signal now corresponding to both analytes. The monochromators were
tuned at 260 (excitation) and 415 (emission) nm, respectively. The calibration graph for salicylamide is linear over the range
0.01 to 0.32 μg mL–1 and for salicylic acid from 0.04 to 1.0 μg mL–1 in the presence of each other. The relative standard deviation and the sampling frequency for the determination of salicylamide
(0.20 μg mL–1) and salicylic acid (0.50 μg mL–1) were 1.1% and 35 h–1, and 0.9% and 45 h–1, respectively. Good results on application to individual determination or mixture resolution in pharmaceutical samples testify
to the usefulness of the proposed sensor.
Received: 20 April 1999 / Revised: 7 June 1999 / Accepted: 12 June 1999 相似文献
19.
Summary Direct chiral-phase HPLC methods have been developed for the determination of flurbiprofen and its major metabolites, namely
4′-hydroxyflurbiprofen and 3′-hydroxy-4′-methoxyflurbiprofen, in biological fluids using a derivatized amylose chiral stationary
phase (CSP; Chiral-pak AD). Quantification of all three analytes, both free and conjugated, in urine was carried out following
liquid-liquid extraction using tandem ultraviolet (UV) and fluorescence detection. Determination of flurbiprofen and the 4′-hydroxy-metabolite
in plasma utilized the same CSP but required modification in the mobile phase composition and sole use of fluorescence detection.
The urine assay was linear (r>0.998) between 0.05–10 μg mL−1, 0.1–20 μg mL−1 and 0.01–2 μg mL−1 for the enantiomers of flurbiprofen, 4′-hydroxyflurbiprofen and 3′-hydroxy-4′-methoxyflurbiprofen respectively. The plasma
assay was linear (r>0.997) between 0.1–6 μg mL−1 and 0.01–0.6 μg mL−1 for the enantiomers of flurbiprofen and 4′-hydroxyflurbiprofen respectively. Both assays, typically yielded within- and between-day
imprecision and accuracy values less than 10% for the enantiomers of the different analytes. Initial volunteer studies suggest
that the disposition of flurbiprofen displays modest enantioselectivity in humans. 相似文献
20.
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