共查询到20条相似文献,搜索用时 31 毫秒
1.
Carlos F. Pedroso Julcemara G. de Oliveira Francinete R. Campos Alan G. Gon?alves Angela C. L. B. Trindade Roberto Pontarolo 《Chromatographia》2009,69(Z2):201-206
A simple RP–LC method for simultaneous quantification of losartan and amlodipine and separation of their degradation products
has been developed. For this purpose we tested appropriated mobile phase pH range, flow rate, temperature and different columns.
The method was validated with an ODS column. A gradient of acetonitrile and phosphate pH 3.0 buffer was utilized as mobile
phase. The linearity was determined at 50–150% level. Individual recoveries at 70–130% level ranged from 98.8 to 100.5% for
losartan and 96.4–101.2% for amlodipine. The robustness was also evaluated. Although losartan has much higher quantities than
amlodipine in commercial tablets, this method allowed simultaneous quantification for both drugs. 相似文献
2.
Stefany Grutzmann Arcari Katia Arena Jeferson Kolling Paloma Rocha Paola Dugo Luigi Mondello Francesco Cacciola 《Electrophoresis》2020,41(20):1784-1792
This study aimed to evaluate the polyphenolic composition along with the biological activity of guabiroba (Campomanesia xanthocarpa Berg.) fruits using comprehensive two-dimensional liquid chromatography (LC × LC). A simplex centroid design comprising three solvents (methanol, 2% acetic acid, and acetonitrile) was used to optimize the extraction mixture for polyphenols from ripe and unripe guabiroba fruits. A quantitative LC × LC platform was proposed to characterize the guabiroba extracts using a RP-Amide column and a C18 column in the first and second dimensions, respectively. Antidiabetic properties, using in vitro enzyme assay models and in vivo antioxidant activity with the eukaryote model Saccharomyces cerevisiae, was measured. Total phenolics compounds were more efficiently extracted with 2% acetic acid solution and acetonitrile (50:50, v/v). A total of 37 different compounds were identified and quantified using the proposed LC × LC method (linearity ranging from 0.9990 to 0.9994, intra- and interday precision from 0.40 to 10.57% and, accuracy from 81.89 to 108.98%). Significant differences were observed between ripe and unripe guabiroba fruits, especially for the compounds geraldone and methyl galangin isomer. Guabiroba fruits showed significant antidiabetic and antioxidant properties and may be potentially adopted as part of dietary strategies in the management of early stages of type 2 diabetes and associated complications. 相似文献
3.
P. López S. Martello A. M. Bermejo Eleonora De Vincenzi M. J. Tabernero M. Chiarotti 《Analytical and bioanalytical chemistry》2010,397(4):1539-1548
This article describes an easy and innovative extraction procedure for cocaine and its primary metabolite, benzoylecgonine
(BE), from hair consisting of sonication with H2O/0.1% formic acid for 4 h. The same extract was used for screening with an enzyme-linked immunoassay (ELISA) and confirmation
by liquid chromatography–tandem mass spectrometry (LC–MS/MS). For the ELISA screening test a cutoff of 0.5 ng/mg was used
according to the Society of Hair Testing recommendations. LC–MS/MS limits of detection (LODs) were established to be 10 pg/mg
and 1 pg/mg for cocaine and BE, respectively. Linearity was obtained over a range of 0.2–5 ng/mg for BE (target analyte) in
the ELISA screening test, while in the LC–MS/MS method the range was 0.10–10 ng/mg for cocaine and 0.01–10 ng/mg for BE. Intra-
and interbatch coefficients of variation and mean relative errors were less than 20% for all analytes and concentrations studied.
The validated ELISA and LC–MS/MS methods were applied to 48 hair samples and the results of both methods were compared; ELISA
demonstrated a sensitivity and specificity of 89.2% and 10.8%. 相似文献
4.
Zhao J Han X Zhao X Wang C Li Q Chen X Bi K 《Analytical and bioanalytical chemistry》2011,401(1):289-296
A liquid chromatographic–mass spectrometric (LC–MS) method has been developed and validated for simultaneous determination
of dehydroevodiamine and limonin from Evodia rutaecarpa in rat plasma. After addition of the internal standard, domperidone, plasma samples were extracted by liquid–liquid extraction
with ethyl acetate and separated on an Apollo C18 column (250 mm × 4.6 mm, 5 μm), with methanol–0.01% formic acid water (60:40, v/v) as mobile phase, within a runtime of 12.0 min. The analytes were detected without interference in the selected ion monitoring
(SIM) mode with positive electrospray ionization. The linear range was 1.0–500 ng mL−1 for dehydroevodiamine and 2.0–1,000 ng mL−1 for limonin, with lower limits of quantitation of 1.0 and 2.0 ng mL−1, respectively. Intra-day and inter-day precision were within 6.0% and 10.9%, respectively, for both analytes, and the accuracy
(relative error, RE, %) was less than 4.8% and 6.5%, respectively. The validated method was successfully applied to a comparative
pharmacokinetic study of dehydroevodiamine and limonin in rat plasma after oral administration of dehydroevodiamine, limonin,
and an aqueous extract of Evodiae fructus. The results indicated there were obvious differences between the pharmacokinetic behavior after oral administration of an
aqueous extract of Evodiae fructus compared with single substances. 相似文献
5.
Miles DR Mesfin M Mody TD Stiles M Lee J Fiene J Denis B Boswell GW 《Analytical and bioanalytical chemistry》2006,385(2):345-356
Liquid chromatography–fluorescence (LC–FLS), liquid chromatography–tandem mass spectrometry (LC–MS/MS) and inductively coupled
plasma–mass spectrometry (ICP-MS) methods were developed and validated for the evaluation of motexafin gadolinium (MGd, Xcytrin)
pharmacokinetics and biodistribution in plasma and tissues. The LC–FLS method exhibited the greatest sensitivity (0.0057 μg
mL−1), and was used for pharmacokinetic, biodistribution, and protein binding studies with small sample sizes or low MGd concentrations.
The LC–MS/MS method, which exhibited a short run time and excellent selectivity, was used for routine clinical plasma sample
analysis. The ICP–MS method, which measured total Gd, was used in conjunction with LC methods to assess MGd stability in plasma.
All three methods were validated using human plasma. The LC–FLS method was also validated using plasma, liver and kidneys
from mice and rats. All three methods were shown to be accurate, precise and robust for each matrix validated. For three mice,
the mean (standard deviation) concentration of MGd in plasma/tissues taken 5 hr after dosing with 23 mg kg−1 MGd was determined by LC–FLS as follows: plasma (0.025±0.002 μg mL−1), liver (2.89±0.45 μg g−1), and kidney (6.09±1.05 μg g−1). Plasma samples from a subset of patients with brain metastases from extracranial tumors were analyzed using both LC–MS/MS
and ICP–MS methods. For a representative patient, ≥90% of the total Gd in plasma was accounted for as MGd over the first hour
post dosing. By 24 hr post dosing, 63% of total Gd was accounted for as MGd, indicating some metabolism of MGd. 相似文献
6.
H. G. Gika F. Michopoulos D. Divanis S. Metalidis P. Nikolaidis G. A. Theodoridis 《Analytical and bioanalytical chemistry》2010,397(6):2191-2197
A 13-min LC–MS method was developed for the determination of daptomycin, a new potent antibiotic, in peritoneal fluid, blood
plasma, and urine of patients receiving renal replacement therapy. Chromatography was performed on a C18 column and detection was performed by a single-quadrupole mass spectrometer coupled to LC via an electrospray interface (ESI).
The column effluent was also monitored at 370 nm using a photodiode-array detector. The developed method provided a linear
dynamic range for concentrations from 0.5 μg mL−1 to 100 μg mL−1. Method precision and accuracy were found to be satisfactory for clinical application, thus the method was successfully used
for the analysis of daptomycin in pharmacokinetic studies. The drug was preventively administered against Gram-positive infections
to 19 clinical patients undergoing peritoneal dialysis. Peritoneal fluid, blood plasma, and urine samples were collected at
13 time points over a period of 48 h. Clinical samples were analysed following simple sample-preparation procedures and daptomycin
was unambiguously detected and quantified. 相似文献
7.
Edith Cristina Laignier Cazedey Débora Pess?a Perez Jaqueline Pess?a Perez Hérida Regina Nunes Salgado 《Chromatographia》2009,69(Z2):241-244
The objective of the current study was to develop and subsequently validate a simple, sensitive and precise reversed-phase
LC method for the determination of ciprofloxacin hydrochloride in ophthalmic solution form. The chromatographic separation
of ciprofloxacin hydrochloride was achieved on a Symmetry Waters C18 column using UV detection at 275 nm. The optimized mobile phase consisted of 2.5% acetic acid solution: methanol:acetonitrile
(70:15:15, v/v/v). The proposed method provided linear responses within the concentration range 1.0–6.0 μg mL−1 for ciprofloxacin hydrochloride. Correlation coefficient (r) for the ciprofloxacin hydrochloride was 0.9994. The precision of the method was demonstrated using intra- and inter-day
assay RSD% values which were less than 5% in all instances. No interference from any components of pharmaceutical dosage forms
was observed. 相似文献
8.
Muñiz-Valencia R Ceballos-Magaña SG Rosales-Martinez D Gonzalo-Lumbreras R Santos-Montes A Cubedo-Fernandez-Trapiella A Izquierdo-Hornillos RC 《Analytical and bioanalytical chemistry》2008,392(3):523-531
An isocratic LC method for the determination of melamine and its degradation products (ammelide, ammeline, and cyanuric acid),
used to increase the apparent protein content of rice protein concentrate, has been developed. Method development involved
optimization of different RP columns, aqueous mobile phases, pH, phosphate concentration, and temperature. The optimum separation
of these compounds was achieved using a Luna CN column (30 °C), 5 mmol L−1 sodium phosphate (pH 5.0) as mobile phase, 1 mL min−1 flow-rate, UV absorbance-DAD detection at 220 nm, and resorcine as internal standard; this enabled separation of these compounds
with baseline resolution (values in the 2.1–10.1 range) in about 8 min. Prior to HPLC, the developed sample preparation procedure
consisted in a leaching process using the above mentioned mobile phase. Method validation was carried out in rice protein
concentrates in accordance with the European Commission decision 2002/657/EC criteria. For this purpose, eight mandatory performance
characteristics for the conventional validation approach were determined: calibration graphs, extraction efficiencies, decision
limits, detection capabilities, precision (repeatability and within-laboratory reproducibility), accuracy, selectivity, and
robustness. The extraction efficiencies for these compounds were in the range 99–100% and the within-laboratory reproducibility
at 1.0, 1.5, and 2.0 detection capabilities concentration levels were smaller than 5, 4, and 3%, respectively. Finally, the
proposed method was successfully applied to the analysis of other rice protein concentrates and several animal feed samples. 相似文献
9.
Mol HG Rooseboom A van Dam R Roding M Arondeus K Sunarto S 《Analytical and bioanalytical chemistry》2007,389(6):1715-1754
The ethyl acetate-based multi-residue method for determination of pesticide residues in produce has been modified for gas
chromatographic (GC) analysis by implementation of dispersive solid-phase extraction (using primary–secondary amine and graphitized
carbon black) and large-volume (20 μL) injection. The same extract, before clean-up and after a change of solvent, was also
analyzed by liquid chromatography with tandem mass spectrometry (LC–MS–MS). All aspects related to sample preparation were
re-assessed with regard to ease and speed of the analysis. The principle of the extraction procedure (solvent, salt) was not
changed, to avoid the possibility invalidating data acquired over past decades. The modifications were made with techniques
currently commonly applied in routine laboratories, GC–MS and LC–MS–MS, in mind. The modified method enables processing (from
homogenization until final extracts for both GC and LC) of 30 samples per eight hours per person. Limits of quantification
(LOQs) of 0.01 mg kg−1 were achieved with both GC–MS (full-scan acquisition, 10 mg matrix equivalent injected) and LC–MS–MS (2 mg injected) for
most of the pesticides. Validation data for 341 pesticides and degradation products are presented. A compilation of analytical
quality-control data for pesticides routinely analyzed by GC–MS (135 compounds) and LC–MS–MS (136 compounds) in over 100 different
matrices, obtained over a period of 15 months, are also presented and discussed. At the 0.05 mg kg−1 level acceptable recoveries were obtained for 93% (GC–MS) and 92% (LC–MS–MS) of pesticide–matrix combinations. 相似文献
10.
This paper describes the validation of an isocratic LC method for the assay of linezolid in tablets. Validation parameters
such as linearity, precision, accuracy, specificity, limit of detection, limit of quantitation and robustness were determined.
LC was carried out by reversed phase technique on an RP-18 column with a mobile phase composed of 1% acetic acid:methanol:acetonitrile
(50:25:25, v/v/v). Linezolid and your combination drug product were exposed to acid, base, oxidation, dry heat and photolytic stress conditions.
A linear response (r > 0.9999) was observed in the range of 8.0–20.0 μg mL−1. The retention time of linezolid was 4.6 min. The method showed good recoveries and intra- and inter-day relative standard
deviations were less than 1.0%. The LOD and LOQ were 0.21 and 0.63 μg mL−1, respectively. The developed LC method for determination of related substances and assay determination of linezolid can be
used to evaluate the quality of regular production samples. It can also be used to test the stability samples of linezolid. 相似文献
11.
Simone Schiesel Michael Lämmerhofer Wolfgang Lindner 《Analytical and bioanalytical chemistry》2010,396(5):1655-1679
The presented work deals with the development and comprehensive validation of a quantitative LC–electrospray ionization (ESI)–tandem
mass spectrometry (MS/MS) method using a triple quadrupole instrument in the MRM mode for the metabolic profiling of amino
acids, organic acids, vitamins, some biogenic amines, secondary metabolites of β-lactam antibiotics biosynthesis as well as
their intermediates, and degradation products in fermentation broths of β-lactam antibiotics production (in total 57 hydrophilic
compounds). A great number of chromatographic systems (22 different stationary phase/mobile phase conditions) were screened
for their adequate chromatographic selectivity to cope with isobaric compounds and other critical analyte pairs. Finally,
a hydrophilic interaction liquid chromatography (HILIC) method employing a zwitterionic ZIC-HILIC column was selected as best
compromise. Particular focus was given on the elucidation of absolute and relative matrix effects via comparison of slopes
of calibration functions of spiked matrix and standard solutions. These data as well as precision and accuracy data confirm
suitability of the HILIC–ESI–MS/MS assay for metabolic profiling studies in fermentation samples. Detailed comprehensive data
sets are presented which should illustrate critical issues, problems, and challenges of multitarget quantitative metabolic
profiling and should outline possible strategies to circumvent pitfalls and overcome common problems. 相似文献
12.
A convenient, selective and sensitive liquid chromatographic-electrospary ionization mass spectrometry (LC–ESI–MS) method
was developed and validated to determine lovastatin in human plasma. The analyte was extracted from human plasma samples by
typical liquid–liquid extraction, separated on a C18 column by using the mobile phase consisting of water–methanol (13:87, v/v). Simvastatin was used as the internal standard (IS). The method was linear within the range of 0.1–20 ng mL−1. The lower limit of quantification (LLOQ) was 0.1 ng mL−1. The intra- and inter-run precision, calculated from quality control (QC) samples was less than 10.2%. The accuracy as determined
from QC samples was in the range of 99.3–102.9% for the analyte. The mean recoveries for lovastatin and IS were 84.8 and 88.0%,
respectively. The method was successfully applied for evaluation of the pharmacokinetic of lovastatin in healthy volunteers. 相似文献
13.
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
14.
Ana Fortuna Joana Sousa Gilberto Alves Amílcar Falcão Patrício Soares-da-Silva 《Analytical and bioanalytical chemistry》2010,397(4):1605-1615
For the first time, a simple, selective and accurate high-performance liquid chromatography method with ultraviolet detection
was developed and validated to quantify simultaneously three structurally related antiepileptic drugs; carbamazepine, oxcarbazepine,
and the recently launched eslicarbazepine acetate and their main metabolites, carbamazepine-10,11-epoxide, 10,11-trans-dihydroxy-10,11-dihydro-carbamazepine, and licarbazepine. The method involves a solid-phase extraction and a reverse-phase
C18 column with 5 cm length. The mobile phase consisting of water, methanol, and acetonitrile in the ratio 64:30:6 was selected
as the best one and pumped at 1 mL/min at 40 °C. The use of this recent column and an aqueous mobile phase instead of buffers
gives several advantages over the method herein developed; namely the fact that the chromatographic analysis takes only 9 min.
The method was validated according to the guidelines of the Food and Drug Administration, showing to be accurate (bias within
±12%), precise (coefficient variation <9%), selective and linear (r
2 > 0.997) over the concentration range of 0.05–30 μg/mL for carbamazepine; 0.05–20 μg/mL for oxcarbazepine; 0.15–4 μg/mL for
eslicarbazepine acetate; 0.1–30 μg/mL for carbamazepine-10,11-epoxide; 0.1–10 μg/mL for 10,11-trans-dihydroxy-10,11-dihydro-carbamazepine, and 0.1–60 μg/mL for licarbazepine. It was also shown that this method can adequately
be used for the therapeutic drug monitoring of the considered antiepileptic drugs, carbamazepine, oxcarbazepine, eslicarazepine
acetate, and their metabolites. 相似文献
15.
Boguslaw Buszewski Pawel Olszowy Tomasz Ligor Malgorzata Szultka Jacek Nowaczyk Maciej Jaworski Marek Jackowski 《Analytical and bioanalytical chemistry》2010,397(1):173-179
Five adrenolytic drugs have been analyzed by liquid chromatography–mass spectrometry (LC–MS). Samples were prepared by solid-phase
microextraction (SPME) using polypyrrole fibers coated on stainless steel support as an adsorbent for the drugs. Adsorption
efficiencies were 95% and were close for all the drugs investigated. Relative standard deviations (RSD), calculated for samples
prepared in standard solutions, were in the range 2.5–13%, however RSD values for the drugs in human plasma were 2.5–4.5%.
Using LC–MS the limit of detection (LOD) and the limit of quantification (LOQ) were in the ranges 0.11–0.18 and 0.39–0.54 ng mL−1, respectively, for the five drugs. 相似文献
16.
Kenichiro Todoroki Hiroki Hashimoto Tomohiko Mikawa Miki Itoyama Tadashi Hayama Eijiro Kojima Hideyuki Yoshida Hitoshi Nohta Masatoshi Yamaguchi 《Analytical and bioanalytical chemistry》2010,397(6):2409-2416
We developed a fluorous scavenging–derivatization method for reagent peak-free liquid chromatography (LC)–fluorescence analysis
of carboxylic acids. In this method, carboxylic acids were fluorescently derivatized with 1-pyrenemethylamine in the presence
of 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide and 1-hydroxy-1H-benzotriazole. Residual excess unreacted reagent was tagged with 2-(perfluorooctyl)ethyl isocyanate and could be selectively
removed by microfluorous solid-phase extraction before LC analysis. With use of this method, eight fluorescent derivatives
of linear aliphatic carboxylic acids (C1–C8) can be separated within 30 min by reversed-phase LC with gradient elution. In the chromatogram obtained, the fluorous-tagged
unreacted reagent peak is greatly decreased after microfluorous solid-phase extraction and does not interfere with the quantification
of each acid. With use of microfluorous solid-phase extraction with 80% (v/v) aqueous methanol elution, over 99.9% of the
unreacted fluorescent reagent was removed. The detection limits (signal-to-noise ratio of 3) for the carboxylic acids examined
are 2.3–8.0 fmol per 10-μL injection. We also applied this method successfully to the analysis of highly polar carboxylic
acids such as α-keto acids and tricarboxylic acid cycle metabolites. 相似文献
17.
Two methods were developed for the quantitative analysis of phenolic acids in herb extracts. The methods were based on liquid
chromatography–time-of-flight mass spectrometry (LC–TOFMS) and gas chromatography–mass spectrometry (GC–MS). The methods were
compared in terms of their linearity, repeatability, selectivity, sensitivity and the speed of the analysis. The sensitivity
was good for both methods, with limits of detection of <80 ng/ml for most of the compounds. The relative standard deviations
(RSD) of the peak areas were on average 7.2% for the LC–TOFMS method and 1.4% for the GC–MS method. Both methods were found
to be suitable for the determination of the target analytes, although GC–MS was better suited to the quantitative determination
of compounds present at low concentrations. 相似文献
18.
Lina Kantiani Marinella Farré Josep Manuel Grases i Freixiedas Damià Barceló 《Analytical and bioanalytical chemistry》2010,398(3):1195-1205
A fully automated method has been developed for analysis of eighteen antibacterial compounds, including penicillins, cephalosporins
and sulfonamides, in animal feed with limits of quantification in the range 0.25–5.79 μg kg−1. The method is based on pressurized liquid extraction of 3 g homogenized feed with water and online clean-up of 500 μL of
the extract with C18HD cartridges. The purified sample was directly analysed by liquid chromatography–electrospray tandem mass spectrometry (SPE–LC–ESI-MS–MS).
Chromatographic separation was achieved within 10 min by use of a C12 Phenomenex Hydro-RP reversed-phase analytical column and a mobile phase gradient (water + 0.1% formic acid–methanol + 0.1%
formic acid). The method was validated, revealing capability for detection of concentrations as low as 0.09 μg kg−1, decision limits (CCα) and detection capabilities (CCβ) in the range 10–174 μg kg−1 and 22–182 μg kg−1, respectively, and inter-day precision ranging from 0.7 to 8.3%. Recovery, with internal standard correction, was in the
range 93–134% for all analytes. The method was then applied to analysis of fifteen feed samples, nine of which contained at
least one antimicrobial at concentrations between 0.006 and 1.526 mg kg−1. The performance data and results from the method were compared with those from a previous method developed by our group,
using offline SPE, by analyzing the same set of samples by both methods. The online SPE approach resulted in slightly improved
sensitivity, with LODs of 0.09–2.12 μg kg−1 compared with 0.12–3.94 μg kg−1 by the offline approach. In general, better recovery was achieved by use of online purification (for 72% of the analytes)
and the correlation between the two methods was good. The main advantages of the new online method are rapid and automated
sample pre-treatment, and reduction of sample manipulation, enabling high-throughput analysis and highly accurate results.
Because of all these characteristics, the proposed method is applicable and could be deemed necessary within the field of
food control and safety. 相似文献
19.
Summary An isocratic, reversed-phase liquid chromatographic (LC) method has been developed for the simultaneous determination of azelaic
and benzoic acids in pharmaceutical creams. The compounds were separated on a C18 column (4 μm particles); the mobile phase was methanolwater, 40∶60, containing 10mm ammonium acetate and with the pH adjusted to 5.0. Detection was performed at 220 nm. The method was validated for accuracy,
linearity, precision, and selectivity. Recoveries at levels corresponding to 80% to 120% of the declared content of the creams
ranged from 99.5 to 101.8% and from 100.4 to 102.1% for azelaic and benzoic acids, respectively. The calibration graphs were
linear in the ranges 20–1400 μg mL−1 for azelaic acid (correlation coefficient,r
1>0.99999), and 0.1–7.0 μg mL−1 for benzoic acid (r>0.99998). 相似文献
20.
This study presents a high-performance liquid chromatography–electrospray ionization–mass spectrometric (LC–ESI–MS) method
for the simultaneous determination of tramadol and acetaminophen in human plasma using phenacetinum as the internal standard.
After alkalization with saturated sodium bicarbonate, both compounds were extracted from human plasma with ethyl acetate and
were separated by HPLC on a Hanbon LiChrospher CN column with a mobile phase of 10 mM ammonium acetate buffer containing 0.5%
formic acid–methanol (40:60, v/v) at a flow rate of 1 mL min−1. Analytes were determined using electrospray ionization in a single quadrupole mass spectrometer. LC–ESI–MS was performed
in the positive selected-ion monitoring (SIM) mode using target ions at [M+H]+
m/z 264.3 for tramadol, [M+H]+
m/z 152.2 for acetaminophen and [M+H]+
m/z 180.2 for phenacetinum. Calibration curves were linear over the range of 5–600 ng mL−1 for tramadol and 0.03–16 μg mL−1 for acetaminophen. The inter-run relative standard deviations were less than 14.4% for tramadol and 12.3% for acetaminophen.
The intra-run relative standard deviations were less than 9.3% for tramadol and 7.9% for acetaminophen. The mean plasma extraction
recovery for tramadol and acetaminophen were in the ranges of 82.7–85.9 and 83.6–85.3%. The method was applied to study the
pharmacokinetics of a new formulation of tramadol/acetaminophen tablet in healthy Chinese volunteers. 相似文献