共查询到20条相似文献,搜索用时 406 毫秒
1.
Xiao-Li Liu Hong-Fang Zhang Guang-Jun Qiao Wei Cao Jian-Bin Zheng 《Chromatographia》2008,67(1-2):147-150
A rapid, sensitive, and specific method for quantification of olmesartan, the prodrug of olmesartan medoxomil, in human plasma,
using zidovudine as internal standard, is described. Sample preparation involved a simple solid-phase extraction procedure.
The extract was analyzed by high-performance liquid chromatography coupled to electrospray tandem mass spectrometry (LC–MS–MS).
Chromatography was performed isocratically on a 5 μm C18 analytical column (50 mm × 4.6 mm i.d.) with water–acetonitrile–formic acid 20:80:0.1 (v/v) as mobile phase. The response to olmesartan was a linear function of concentration over the range 4.82–1,928 ng mL−1. The lower limit of quantification in plasma was 4.82 ng mL−1. The method was successfully applied in a bioequivalence study of an olmesartan formulation after administration as a single
oral dose. 相似文献
2.
Babu Rao Chandu Sreekanth Nama Kanchanamala Kanala Balasekhara Reddy Challa Rihana Parveen Shaik Mukkanti Khagga 《Analytical and bioanalytical chemistry》2010,398(3):1367-1374
A novel simple, sensitive, selective, and rapid high-performance liquid chromatography coupled with tandem mass spectrometry
method was developed and validated for quantification of riluzole in human plasma. The chromatography was performed by using
a Zorbax-SB-C18 (4.6 × 75 mm, 3.5 μm) column , isocratic mobile phase 0.1% formic acid/acetonitrile (10:90 v/v), and an isotope-labeled
internal standard (IS), [13C,15N2]riluzole. The extraction of drug and internal standard was performed by liquid–liquid extraction and analyzed by MS in the
multiple reaction monitoring (MRM) mode using the respective [M+H]+ ions, m/z 235.0/165.9 for riluzole and m/z 238.1/169.0 for the IS. The calibration curve was linear over the concentration range 0.5–500.0 ng/ml for riluzole in human
plasma. The limit of quantification (LOQ) was demonstrated at 0.5 ng/ml. The within-batch and between-batch precision were
0.6–2.3% and 1.4–5.7%, and accuracy was 97.1–101.1% and 98.8–101.2% for riluzole respectively. Drug and IS were eluted within
3.0 min. The validated method was successfully applied in a bioequivalence study of riluzole in human plasma. 相似文献
3.
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
4.
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
5.
A simple high-performance liquid chromatographic method was developed for determining five major components of teicoplanin,
designated A2–1, A2–2, A2–3, A2–4 and A2–5, in human plasma. Using piperacillin sodium as internal standard, teicoplanin in
plasma samples was extracted by coextractive cleanup procedure. The extracts were injected into a Nova-Pak C18 column maintained at ambient temperature. The mobile phase consisted of acetonitrile–0.1% trifluoroacetic acid (27:73, pH = 2.2),
at a flow rate of 1.0 mL min−1. The analytes were detected at the UV wavelength of 218 nm. The method was found to be linear over the concentration range
of 2.5–50 mg L−1 for teicoplanin (r = 0.9993 ± 0.0038), which covered the clinically expected trough plasma levels. The percentage error of the analytical method
was below 9%. The intra- and inter-day reproducibility was adequate with coefficients of variation less than 7%. The chromatographic
running time was 11 min. Thus, the method can be effectively applied to measure teicoplanin concentrations in clinical samples. 相似文献
6.
dos Santos EJ Herrmann AB Frescura VL Welz B Curtius AJ 《Analytical and bioanalytical chemistry》2007,388(4):863-868
Among the “traditional” hydride-forming elements, lead is probably the most difficult, and its determination in this form
has rarely been reported in the literature. In this paper a simple and rapid method, axial-view inductively-coupled plasma
optical-emission spectrometry using on-line hydride generation (HG–ICP–OES) from samples prepared as slurry, is proposed for
determination of lead in environmental samples. The samples (20–50 mg, particle size ≤120 μm) were treated with 1 mL aqua
regia in a 40-kHz ultrasonic bath for 60 min. The slurry was diluted to a final volume of 50 mL with a 10% m/v solution of (NH4)2S2O8. The concentrations of NaBH4, tartaric acid, and (NH4)2S2O8, used for on-line plumbane generation were optimized by means of a complete factorial analysis applied to an aqueous standard
solution and to the slurry of a sediment certified reference material (CRM). External calibration against aqueous standards
in the concentration range 10–100 μg L−1 was used for analysis of six CRM—three marine sediments, one river sediment, and two sewage sludges. Analysis of the filtered
slurry showed that Pb was only partially extracted into the liquid phase. Several major concomitants tested did not affect
the Pb signal. The detection limit (3s, n = 10) for 20 mg sample in a final volume of 50 mL was 5.0 μg g−1. Tin was the only other hydride-forming analyte that could be determined satisfactorily with Pb; for tin the detection limit
was 1.0 μg g−1. The values obtained for Pb and Sn were not significantly different from the certified concentrations, according to the t-test at the 95% confidence level. Nine river sediments collected locally were also analyzed and the concentrations were in
agreement with results obtained after total digestion. 相似文献
7.
Jun Wen Zhenyu Zhu Zhanying Hong Yiwen Wu Yan Fei Mei Lin Guorong Fan Yutian Wu 《Chromatographia》2007,66(1-2):37-41
A cheap, simple and rapid sample preparation method has been developed for quantification of ulifloxacin, the active metabolite
of prulifloxacin in human plasma, by HPLC with fluorescence detection using lemefloxacin as the internal standard. One-step
protein precipitation with 10% perchloric acid (2:1, v/v) on a 200 μL sample was used. The separation was performed at 30 °C on a C18 column using an eluent of acetonitrile-0.5%
triethylamine buffer. The compounds were monitored at λ
ex of 280 nm, λ
em of 425 nm. The calibration curve for ulifloxacin in human plasma was linear over the range 0.01–1.00 μg mL−1. The lower limit of quantification is 0.01 μg mL−1. The intra- and inter-day precision ranged from 3.0 to 6.7%, respectively. The method had been used for clinical pharmacokinetic
studies of prulifloxacin formulation product after oral administration to healthy volunteers.
Jun Wen and Zhenyu Zhu have equal contribution to this work. 相似文献
8.
El-Khoury JM Bunch DR Reineks E Jackson R Steinle R Wang S 《Analytical and bioanalytical chemistry》2012,402(2):771-779
Asymmetric dimethylarginine (ADMA) is an endogenous inhibitor of nitric oxide synthase and an established biomarker for endothelial
function, while symmetric dimethylarginine (SDMA), an emerging biomarker for renal function, has been shown to outperform
creatinine-based equations for estimated glomerular filtration rate. In order to study these analytes for clinical research,
a fast and simple method for measuring arginine (ARG), SDMA, and ADMA in plasma by liquid chromatography–tandem mass spectrometry
(LC-MS/MS) has been developed. Plasma (50 μL) was mixed with 50 μL of internal standard of 13C-arginine and d7-ADMA followed by protein precipitation with methanol containing 1% ammonium acetate (300 μL). After centrifugation, the supernatant
(100 μL) was mixed with 300 μL of acetonitrile with 1% formic acid, and the mixture was injected onto a silica column monitored
by a mass spectrometer. The analytical cycle time was 5.0 min. The method was linear from 5.7 to 489.7 μM for ARG, 0.06 to
5.15 μM for SDMA, and from 0.34 to 5.65 μM for ADMA, with an accuracy of 99.0–120.0%. Total coefficients of variation for
all analytes ranged from 2.7% to 7.7% for three concentration levels. The effects of hemolysis, lipemia, uremia, icterus,
specimen tube types, storage at different temperature, and freeze/thaw were thoroughly investigated. Reference ranges were
established using 51 well-defined reference subjects (12 men and 39 women, age 19–64 years): 53.1–129.7 μM for ARG, 0.32–0.65 μM
for SDMA, and 0.36–0.67 μM for ADMA. In conclusion, the validated LC-MS/MS method described here offers a fast and reliable
ARG, SDMA, and ADMA quantitation in plasma with minimum sample preparation. 相似文献
9.
Summary Elevated plasma homocysteine is, a known risk factor in arteriosclerotic vascular disease. To measure homocysteine in a large
number of samples, we have developed a rapid, simple, robust and inexpensive reversed-phase HPLC method for routine analysis.
Mercaptopro-pionylglycine was used as the internal standard and an external calibration in plasma was performed. Improvement
was achieved by the use of gradient elution (using a sodium acetate buffer and methanol) resulting in a higher number of samples
analyzed per day. Plasma samples were reduced with tributylphosphine and the proteins were precipitated with perchloric acid
before addition of internal standard. The analytes were derivatized by use of 7-fluorobenzofurazone-4-sulfonic acid ammonium
salt. For calibration human plasma was spiked with nine different concentrations of homocysteine (range 2–50 μmol L−1). The inter-assay precision of replicate (n=29) analysis of the concentration of homocysteine in a sample of pooled plasma was 3.0%. The limit of detection, defined
as three times the signal-to-noise ratio, was 0.25 μmol L−1. The linearity of the assay was confirmed for a plasma concentration range of 2–2000 μmol L−1. The variation of duplicate analyses of 842 plasma samples was 2.6±1.7%. 相似文献
10.
A sensitive and selective HPLC–UV method established for determination of picroside I in dog plasma has been used to study
the pharmacokinetics of the drug after intravenous administration of three different doses. Sample pretreatment consists in
deproteination by addition of acetonitrile; l-ascorbic acid was used to improve the stability of picroside I. The lower limit of quantification of picroside I was 0.05 μg mL−1. The recovery of the method was up to 90%. After intravenous administration to dogs picroside I was mainly distributed in
the central compartment and was rapidly eliminated from the plasma; the mean elimination half-life was 30.54 ± 4.34, 30.20 ± 3.78,
and 34.02 ± 1.88 min for doses of 2.5, 5, and 15 mg kg−1, respectively, and the respective values of AUC
0–∞ were 81.04 ± 19.95, 198.50 ± 27.77, and 586.44 ± 103.08 μg min mL−1. The different doses had no significant effect on the main pharmacokinetic data and the kinetics seemed to be linear in dosage
range 2.5–15 mg kg−1. 相似文献
11.
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
12.
Summary A rapid and simple liquid-chromatographic method has been developed for on-line quantification of amphetamine in biological
fluids. Untreated samples (20 μL) are injected directly into the chromatographic system and purified on a 20 mm×2.1 mm i.d.
pre-column packed with 30 μm Hypersil C18 stationary phase. After clean-up the analyte is transferred to the analytical column (125 mm×4 mm i.d., 5 μm LiChrospher
100 RP18) for derivatization and separation using a mixture of acetonitrile and the derivatization reagent (o-phthaldialdehyde andN-acetyl-L-cysteine) as the mobile phase. The experimental conditions for on-line derivatization and resolution of the amphetamine
have been optimized, and the results have been compared with those obtained by derivatizing the analyte in pre-column mode.
The method described has been applied to the determination of amphetamine in plasma and urine. Good linearity and reproducibility
were obtained in the 0.1–10.0 μg mL−1 concentration range, and limits of detection were 25 ng mL−1 and 10 ng mL−1 with UV and fluorescence detection, respectively. The procedure described is very simple and rapid, because no off-line manipulation
of the sample is required; the total analysis time is approximately 8 min. 相似文献
13.
H. M. Lee C. K. Jeong S. J. Choi B. M. Yoon D. H. Na K. C. Lee H. S. Lee 《Chromatographia》2000,51(5-6):353-356
Summary An automated microbore, liquid chromatographic method with column-switching was developed for the determination of clomipramine
from human plasma samples. After direct injection of samples (60 μL), plasma proteins and clomipramine were separated in size-exclusion
mode using 20% acetonitrile in 20 mM phosphate buffer (pH 7.0) on Capcell Pak MF Ph-1 precolumn (10×4 mm I.D.). By valve switching,
a fraction containing clomipramine was directed to an intermediate column for subsequent main separation on a microbore C18 column (250×1.5 mm I.D.) using 50% acetonitrile in 20 mM phosphate buffer (pH 2.5) at 0.1 mL min−1. The method was advantageous for rapidity (total analysis time: 15 min), reproducibility (C.V.<4.8%), and increased sensitivity
(1 ng mL−1). The linearity of response was good (r
2≥0.999) over the concentration range 1–250 ng mL−1. 相似文献
14.
Authors developed a simple, sensitive, selective, rapid, rugged, and reproducible liquid chromatography–tandem mass spectrometry
method for the quantification of eletriptan (EP) in human plasma using naratriptan (NP) as an internal standard (IS). Chromatographic
separation was performed on Ascentis Express C18, 50 × 4.6 mm, 2.7 μm column. Mobile phase was composed of 0.1% formic acid:
methanol (40:60 v/v), with 0.5 mL/min flow rate. Drug and IS were extracted by liquid–liquid extraction. EP and NP were detected with proton
adducts at m/z 383.2→84.3 and 336.2→97.8 in multiple reaction monitoring (MRM) positive mode, respectively. The method was validated with
the correlation coefficients of (r
2) ≥ 0.9963 over a linear concentration range of 0.5–250.0 ng/mL. This method demonstrated intra- and inter-day precision within
1.4–9.2% and 4.4–5.5% and accuracy within 96.8–103% and 98.5–99.8% for EP. This method is successfully applied in the bioequivalence
study of 24 human volunteers. 相似文献
15.
High performance liquid chromatography method for the determination of meropenem in human plasma 总被引:2,自引:0,他引:2
Summary This paper describes an HPLC method for the determination of meropenem in human plasma. The method uses solid phase extraction
(SPE) of the samples and has good sensitivity, precision and accuracy. The limit of quantification in plasma samples is 0.02
μg mL−1. Calibration curves were linear over a large dynamic range, namely within 0.02–50 μg mL−1. The method was applied to the determination of meropenem levels in patients receiving meropenem, as a single dose or at
steady state. 相似文献
16.
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
17.
J. W. Bae C. S. Myung C. I. Choi S. M. Moon C. G. Jang S. Y. Lee 《Journal of Analytical Chemistry》2010,65(12):1261-1265
The purpose of this study was to validate a reliable analytical method for pharmacokinetic study of ceftibuten in human plasma
by high performance liquid chromatography (HPLC) system with UV detection. Ceftizoxime was used as the internal standard.
After plasma sample was precipitated with acetonitrile and dichloromethane, the supernatant was directly injected into the
HPLC system. Separation was performed on a Capcell Pak C18 UG120 column (4.6 mm × 250 mm, 5 μm particles) with a mobile phase of acetonitrile/50 mM ammonium acetate (5: 95, v/v) and
UV detection at a wavelength of 262 nm. The intra- and inter-day precision expressed as the relative standard deviation was
less than 15%. The lower limit of quantification was 0.5 hg/mL of ceftibuten using 0.5 mL of plasma. The calibration curve
was linear in concentration range of 0.5–30 μg/mL (r
2 = 0.9998). The mean accuracy was 96–102%. The coefficient of variation (precision) in the intra- and inter-day validation
was 0.9–3.9 and 0.9–2.4%, respectively. The pharmacokinetics of ceftibuten was evaluated after a single oral administration
of 400 mg to healthy volunteers. The AUC0–9 h, c
max, T
max, and T
1/2 were 86.6 ± 12.7 μg h/mL, 18.4 ± 1.5 μg/mL, 2.63 ± 0.83 and 2.65 ± 0.41 h, respectively. The method was demonstrated to be
highly reproducible and feasible for pharmacokinetic studies of ceftibuten in eight volunteers after oral administration (400
mg as ceftibuten). 相似文献
18.
Yan Liang Jie Sun Lin Xie An Kang Yuan Xie Wei-Dong Chen Hua Lv Guang-Ji Wang 《Chromatographia》2007,66(3-4):165-170
A sensitive and specific liquid chromatographic method with electrospray ionization mass spectrometry (LC–ESI-MS) has been
developed and validated for identification and quantification of mitiglinide in human urine. A simple liquid–liquid extraction
procedure was followed by separation on a C18 column with gradient elution, and detection using a single-quadrupole mass spectrometer in selected-ion-monitoring (SIM)
mode. The method was tested using six different batches of urine. Linearity was established for the mitiglinide concentrations
in the range 0.005–1.0 μg mL−1, with a coefficient of determination (r) of 0.9998 and good back-calculated accuracy and precision. Intra- and inter-day precision (as RSD, %) was below 10% and
accuracy for mitiglinide ranged from 85 to 115%. The lower limit of quantification was reproducible at 0.002 μg mL−1 for 500 μL urine. The proposed method enables unambiguous identification and quantification of mitiglinide in pre-clinical
and clinical studies. 相似文献
19.
A rapid and sensitive high-performance liquid chromatographic (HPLC) assay for the simultaneous determination and quantification
of cefpirome and cetirizine or cefpirome and levocetirizine in pharmaceutical formulations and human plasma without changing
the chromatographic conditions is described. Chromatographic separations were performed on a prepacked Nucleosil 120, C18 (5 μm, 12.5 ± 0.46 mm) column using CH3CN: H2O (75: 25, v/v) as a mobile phase at a flow rate of 1 mL/min while UV detection was performed at 232 nm for monitoring the
effluent. A number of other brands of C18 columns were also employed which had a significant effect on the separation. The method has been validated over the concentration
range of 0.5–50 μg/mL (r
2 > 0.999). The limit of detection (LOD) and quantification (LOQ) for cefpirome and levocetirzine in pharmaceutical formulations
and serum were in the range 0.24–1.31 μg/mL. Analytical recovery from human plasma was >98%, and the within and between-day
relative standard deviation was <3.1%. The small sample volume and simplicity of preparation make this method suitable for
use in pharmaceutical industries, drug research centers, clinical laboratories, and forensic medical centers.
The text was submitted by the authors in English. 相似文献
20.
Summary A sensitive and selective high-performance liquid chromatographic method has been developed for monitoring clozapine levels
in human plasma. Chromatography was performed on a reversed-phase column (C8, 150 mm×4.6 mm i.d., 5 μm) with acetonitrile-aqueous sodium acetate solution, 88∶12 (v/v), as mobile phase; the flow rate was 1 mL min−1. Clozapine oxidation at +800 mV was detected amperometrically. Response was linearly dependent on concentration over the
range 50–1500 ng mL−1 clozapine in plasma. Sample preparation by solid-phase extraction before HPLC analysis gave high extraction yield (94%).
The accuracy and precision of the method were both very good (recovery: 97%;RSD<3.3%). 相似文献