共查询到20条相似文献,搜索用时 562 毫秒
1.
A sensitive, simple, and accurate high-performance liquid chromatographic method has been developed for determination of valdecoxib and the internal standard rofecoxib in human plasma. Protein was precipitated from plasma samples by addition of perchloric acid (HClO4); the drug was then extracted with diethyl ether. Separation was performed on a Cosmosil C18 column (150 mm × 4.6 mm i.d., 5 m particles) with ammonium acetate buffer-acetonitrile, 60:40 (v/v), containing 0.1% TEA, pH 6.5, as mobile phase. Detection and quantification were performed by UV-visible detection at 239 nm. Detection and quantification limits were 3 and 5 ng mL–1, respectively. The linear concentration range for valdecoxib was 5–400 ng mL–1. The validated RP HPLC method was used for determination of the pharmacokinetic data for the drug in humans. 相似文献
2.
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
3.
Lawrence Asamoah Adutwum Naoya Kishikawa Kaname Ohyama Shiro Harada Kenichiro Nakashima Naotaka Kuroda 《Analytical and bioanalytical chemistry》2010,398(2):823-829
A sensitive and selective high performance liquid chromatography-peroxyoxalate chemiluminescence (PO-CL) method has been developed
for the simultaneous determination of chlorpheniramine (CPA) and monodesmethyl chlorpheniramine (MDCPA) in human serum. The
method combines fluorescent labeling with 4-(4,5-diphenyl-1H-imidazole-2-yl)phenyl boronic acid using Suzuki coupling reaction with PO-CL detection. CPA and MDCPA were extracted from
human serum by liquid–liquid extraction with n-hexane. Excess labeling reagent, which interfered with trace level determination of analytes, was removed by solid-phase
extraction using a C18 cartridge. Separation of derivatives of both analytes was achieved isocratically on a silica column
with a mixture of acetonitrile and 60 mM imidazole-HNO3 buffer (pH 7.2; 85:15, v/v) containing 0.015% triethylamine. The proposed method exhibited a good linearity with a correlation coefficient of 0.999
for CPA and MDCPA within the concentration range of 0.5–100 ng/mL. The limits of detection (S/N = 3) were 0.14 and 0.16 ng/mL
for CPA and MDCPA, respectively. Using the proposed method, CPA could be selectively determined in human serum after oral
administration. 相似文献
4.
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
5.
This contribution describes use of a separation method based on on-line coupling of a multisyringe flow system with a chromatographic
monolithic column for simultaneous determination of hydrochlorothiazide and losartan potassium in tablets. The system comprised
a multisyringe module, three low-pressure solenoid valves, a monolithic C18 column (25 mm × 4.6 mm i.d.), and a diode-array detector. The mobile phase was 10 mmol L−1 potassium dihydrogen phosphate (pH 3.1)-acetonitrile-methanol (65:33:2 v/v/v) at a flow rate 0.8 mL min−1. UV detection was carried out at 226 nm. The multi-syringe chromatographic (MSC) method with UV spectrophotometric detection
was optimized and validated. Results from validation were very good. The analysis time was about 400 s. The method was found
to be applicable to routine analysis of both compounds in tablets. The coupling of the monolithic columns with a multi-syringe
flow-injection analysis manifold provides an excellent and inexpensive tool to solve the separation problems without use of
HPLC instrumentation. 相似文献
6.
Wietecha-Posłuszny R Garbacik A Woźniakiewicz M Kościelniak P 《Analytical and bioanalytical chemistry》2011,399(9):3233-3240
The objective of this research was to develop, optimize, and validate a modern, rapid method of preparation of human hair
samples, using microwave irradiation, for analysis of eight tricyclic antidepressants (TCADs): nordoxepin, nortriptyline,
imipramine, amitriptyline, doxepin, desipramine, clomipramine, and norclomipramine. It was based on simultaneous alkaline
hair microwave-assisted hydrolysis and microwave-assisted extraction (MAH–MAE). Extracts were analyzed by high-performance
liquid chromatography with diode-array detection (HPLC–DAD). A mixture of n-hexane and isoamyl alcohol (99:1, v/v) was used as extraction solvent and the process was performed at 60°C. Application of 1.0 mol L−1 NaOH and microwave irradiation for 40 min were found to be optimum for hair samples. Limits of detection ranged from 0.3
to 1.2 μg g−1 and LOQ from 0.9 to 4.0 μg g−1 for the different drugs. This enabled us to quantify them in hair samples within average therapeutic concentration ranges. 相似文献
7.
A weak cation-exchange monolithic column has been prepared in stainless steel tubing and used as the solid-phase extraction
material in quantitative analysis of caffeine and theophylline in urine. Column switching, with water as mobile phase, was
used for on-line cleaning and screening of human urine samples. Reversed-phase high-performance liquid chromatography was
then performed on a C18 column with methanol–water 30:70 (v/v) as mobile phase at a flow rate of 0.5 mL min−1. Ultraviolet detection was performed at 274 nm. Good linear relationships were obtained between response and concentrations
of caffeine and theophylline in the range 0.1–50 μg mL−1. Absolute recovery ranged from 77.4 to 82.3% and inter-day and intra-day relative standard deviations were less than 5%.
The method was suitable for analysis of caffeine and theophylline in human urine, because it eliminated tedious pretreatment
and enabled rapid, economic, repeatable, and effective assay of traces of the drugs in biological samples. 相似文献
8.
Summary A high-performance liquid chromatographic method with ultraviolet detection has been developed for the analysis of the polypeptide
antibiotic zinc bacitracin in adulterated animal feed. Firstly, the process for extraction of the antibiotic from the feed
was optimized. This process involved extraction from the feed at pH 2, centrifugation, liquid-liquid extraction, then solidphase
extraction. The extract obtained was then dissolved in the mobile phase and injected into the chromatograph. The best analytical
results were obtained by use of a C18 column with a mobile phase comprising a 50:50 (%,v/v) mixture of 0.3m phosphate buffer, pH 3, containing 20mm sodium dodecyl sulfate (SDS) and 19:1 (v/v) acetonitrile-methanol. The analytical signal (peak area) was monitored at 254 nm. The calibration function was estimated
between 200 and 1000 mg L−1. The proposed method was applied to the analysis of zinc bacitracin present in different fortified animal feed products at
levels between 5 and 200 mg kg−1. Recovery rates were between 66 and 85% and the relative standard deviation was below 7%. 相似文献
9.
P. R. Oliveira L. Brum Junior M. Fronza L. S. Bernardi S. M. K. Masiero S. L. Dalmora 《Chromatographia》2006,63(7-8):315-320
An analytical method based on liquid chromatography-tandem mass spectrometry (LC-MS-MS) was developed and validated for the
determination of ezetimibe in human plasma. Ezetimibe and etoricoxib (internal standard) were extracted from the plasma by
liquid-liquid extraction and separated on a C18 analytical column (50 × 3.0 mm I.D.) with acetonitrile:water (85:15, v/v) as mobile phase. Detection was carried out by positive electrospray ionization (ESI+) in multiple reaction monitoring (MRM)
mode. The chromatographic separation was obtained within 2.0 min and was linear in the concentration range of 0.25–20ng mL−1 for free ezetimibe and of 1–300ng mL−1 for total ezetimibe. The mean extraction recoveries for free and total ezetimibe from plasma were 96.14 and 64.11%, respectively.
Method validation investigated parameters such as linearity, precision, accuracy, specificity and stability, giving results
within the acceptable range. The proposed method was successfully applied to the quantitation of ezetimibe and its glucuronide
in human plasma to support clinical and pharmacokinetic studies. Moreover, the method was used for the quality control analysis
of pharmaceutical dosage forms.
Revised: 4 January and 3 February 2006 相似文献
10.
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
11.
Apichai Santalad Supalax Srijaranai Rodjana Burakham Jeremy D. Glennon Richard L. Deming 《Analytical and bioanalytical chemistry》2009,394(5):1307-1317
A cloud-point extraction (CPE) method using Triton X-114 non-ionic surfactant was developed for the extraction and preconcentration
of carbamate insecticide residues (i.e., methomyl, propoxur, carbofuran, carbaryl, isoprocarb, and promecarb) in fruit samples.
The optimum conditions of CPE were 1.5% (w/v) Triton X-114, 7.0% (w/v) NaCl and 20 min equilibrated at 45 °C. The surfactant-rich phase was then analyzed by reversed-phase high-performance liquid
chromatography with ultraviolet detection at 270 nm, under gradient separation using methanol and 0.1% (v/v) acetic acid. Under the study conditions, six carbamate insecticides were successfully separated within 27 min. Good reproducibility
was obtained with the relative standard deviation of <3% for retention time and <9% for peak area. Limits of detection in
the studied fruit samples were in the range of 0.1–1.0 mg kg−1. No carbamate insecticides were detected in the studied fruit samples. The high recoveries of the spiked fruit samples were
obtained in the range 80.0–107%. The CPE method has been shown to be a potential useful methodology for the preconcentration
of the target analytes, with a preconcentration factor of 14. Moreover, the method is simple, has high sensitivity, consumes
much less solvent than traditional methods, and is environmental friendly. 相似文献
12.
Consuelo Cháfer-Pericás Ángel Maquieira Rosa Puchades Javier Miralles Amelia Moreno 《Analytical and bioanalytical chemistry》2010,396(2):911-921
An indirect competitive enzyme-linked immunosorbent assay (ELISA) was developed in plate to detect three sulfonamide residues
(sulfamerazine (SMR), sulfadimetoxine (SDM), and sulfadiazine (SDZ)) in gilthead sea bream (Sparus aurata) samples. Different extraction methodologies—using methanol/water 1:1 (v/v) + ethylene diamine tetraacetic acid (EDTA) 0.5% (m/v), acetonitrile, phosphate-buffered saline (PBS) 10 mmol L−1 pH 7 and acetate buffer 100 mmol L−1 pH 5—and cleanup steps, based on solid-phase extraction (C18, SCX, Si) or liquid extraction with hexane, were assayed. As optimum, a fast and simple method using acetonitrile was selected
to extract the sulfonamide residues from the edible muscle of fish. Due to matrix effects, a standard addition calibration
curve in fish extract is necessary for quantification purposes. Sulfonamide-free samples were spiked at different concentration
levels (between 30 and 90 ng g−1, 5–15 ng mL−1 in plate) and average recoveries (n = 8), ranging from 71% to 95%, 65% to 79%, and 72% to 95%, were obtained for SMR, SDM, and SDZ, respectively. The assay detection
limits for these antibiotics were lower than 100 μg kg−1 (maximum residue level established by the European Union). The accuracy was evaluated by spiking blank fish extracts at different
concentrations (10–40 ng mL−1, 5–20 ng mL−1 in plate), and the relative errors ranged between ±20%. Finally, in order to confirm the utility of the developed ELISA as
a screening methodology, fish samples from different supermarkets were analyzed, and results were compared with those obtained
by a validated high-performance liquid chromatography (HPLC) method. The correlation between the results obtained by both
ELISA and HPLC methods is satisfactory.
相似文献
13.
Viñas P López-García I Bravo-Bravo M Briceño M Hernández-Córdoba M 《Analytical and bioanalytical chemistry》2012,403(4):1059-1066
A miniaturized dispersive liquid–liquid microextraction (DLLME) procedure coupled to liquid chromatography (LC) with fluorimetric
detection was evaluated for the preconcentration and determination of thiamine (vitamin B1). Derivatization was carried out by chemical oxidation of thiamine with 5 × 10−5 M ferricyanide at pH 13 to form fluorescent thiochrome. For DLLME, 0.5 mL of acetonitrile (dispersing solvent) containing
90 μL of tetrachloroethane (extraction solvent) was rapidly injected into 10 mL of sample solution containing the derivatized
thiochrome and 24% (w/v) sodium chloride, thereby forming a cloudy solution. Phase separation was carried out by centrifugation, and a volume of
20 μL of the sedimented phase was submitted to LC. The mobile phase was a mixture of a 90% (v/v) 10 mM KH2PO4 (pH 7) solution and 10% (v/v) acetonitrile at 1 mL min−1. An amide-based stationary phase involving a ligand with amide groups and the endcapping of trimethylsilyl was used. Specificity,
linearity, precision, recovery, and sensitivity were satisfactory. Calibration graph was carried out by the standard additions
method and was linear between 1 and 10 ng mL−1. The detection limit was 0.09 ng mL−1. The selectivity of the method was judged from the absence of interfering peaks at the thiamine elution time for blank chromatograms
of unspiked samples. A relative standard deviation of 3.2% was obtained for a standard solution containing thiamine at 5 ng mL−1. The esters thiamine monophosphate and thiamine pyrophosphate can also be determined by submitting the sample to successive
acid and enzymatic treatments. The method was applied to the determination of thiamine in different foods such as beer, brewer’s
yeast, honey, and baby foods including infant formulas, fermented milk, cereals, and purees. For the analysis of solid samples,
a previous extraction step was applied based on an acid hydrolysis with trichloroacetic acid. The reliability of the procedure
was checked by analyzing a certified reference material, pig’s liver (CRM 487). The value obtained was 8.76 ± 0.2 μg g−1 thiamine, which is in excellent agreement with the certified value, 8.6 ± 1.1 μg g−1. 相似文献
14.
Skalka N Krol A Schlesinger H Altstein M 《Analytical and bioanalytical chemistry》2011,400(10):3491-3504
The present research focused on the development of an immunoassay and an immunochemical sol–gel-based immunoaffinity purification
(IAP) method for purification and detection of the non-steroid anti-inflammatory drug (NSAID) indomethacin (IMT). A polyclonal
antibody (Ab) for IMT was generated, and two sensitive microplate assays for the detection of IMT were developed (termed OV
and HRP formats), based on the enzyme-linked immunosorbent assay (ELISA) method. The limits of detection of the assays were
15 ± 1.25 ng mL−1 (n = 50) and 12 ± 0.17 ng mL−1 (n = 4) for the OVA and HRP formats, respectively. The Abs exhibited slight cross-reactivity with other NSAIDs. The Abs were
also used to develop a sol–gel-based IAP method for clean-up and concentration of IMT. Several sol–gel formats with various
amounts of antibodies were examined; the best and most reproducible format was at a TMOS:HCl molar ratio of 1:6 in which 120 μL
of IMT Abs was entrapped. The binding capacity under these conditions was ca. 100 to 250 ng of IMT with very low non-specific
binding (less than 5% of the applied amount). The sol–gel IAP method, combined with solid-phase extraction, successfully eliminated
serum interference to a degree that enabled analysis of spiked serum samples by ELISA. The method was also found to be fully
compatible with subsequent chemical analytical methods, such as liquid chromatography followed by mass spectrometry. The approaches
developed in this study form a basis for analysis of IMT in biological samples in order to monitor their pharmacokinetic properties,
and may be further used to study population exposure to IMT, and to monitor the occurrence of IMT contamination in water samples. 相似文献
15.
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
16.
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
17.
Reiter EV Cichna-Markl M Chung DH Shim WB Zentek J Razzazi-Fazeli E 《Analytical and bioanalytical chemistry》2011,400(8):2615-2622
The paper presents a new sample clean-up method based on immuno-ultrafiltration for the analysis of ochratoxin A in cereals.
In contrast to immunoaffinity chromatography, in immuno-ultrafiltration, the antibodies are used in non-immobilised form.
Ochratoxin A was extracted with ACN/water (60/40, v/v), and the extract was loaded onto the ultrafiltration device. After a washing step with phosphate-buffered saline, containing
0.05% Tween 20, ochratoxin A was eluted with MeOH/acetic acid (99/1, v/v). The detection of ochratoxin A was carried out with high-performance liquid chromatography and a fluorescence detector coupled
to an electrochemical cell (Coring cell). The electrochemical cell was used to eliminate matrix interferences by oxidising
matrix compounds. The method was validated by repeatedly analysing spiked barley and rye samples as well as a certified wheat
reference material. Recoveries and standard deviations (1 SD) were found to be 71 ± 9%, 77 ± 12% and 77 ± 8% in wheat, barley
and rye, respectively. The limit of detection (S/N = 3) and limit of quantitation (S/N = 10) were determined to be 0.4 μg kg-1 and 1 μg kg-1. The analysis of the certified reference material resulted in ochratoxin A concentrations which were in the range assigned
by the producer. Additionally, the effect of the electrochemical cell on other widely used clean-up techniques, namely the
immunoaffinity clean-up and multifunctional columns (Mycosep #229), was evaluated. In all clean-up methods, an improvement
of the chromatogram quality was registered. 相似文献
18.
A high-performance liquid chromatographic method with triple-quadrupole mass spectrometry detection (LC-MS-MS) was developed
and validated for the first time for the simultaneous quantification of zopiclone and its metabolites in rat plasma samples.
The analytes were isolated from rat plasma by liquid–liquid extraction and separated using a chiral stationary phase based
on an amylose derivative, Chiralpak ADR-H column, and ethanol–methanol–acetonitrile (50:45:5, v/v/v) plus 0.025% diethylamine as the mobile phase, at a flow-rate of 1.0 mL min−1. Moclobemide was used as the internal standard. The developed method was linear over the concentration range of 7.5–500 ng mL−1. The mean absolute recoveries were 74.6 and 75.7; 61.6 and 56.9; 72.5, and 70.7 for zopiclone enantiomers, for N-desmethyl zopiclone enantiomers and for zopiclone-N-oxide enantiomers, respectively, and 75.9 for the internal standard. Precision and accuracy were within acceptable levels
of confidence (<15%). The method application in a pilot study of zopiclone kinetic disposition in rats showed that the levels
of (+)-(S)-zopiclone were always higher than those of (−)-R-zopiclone. Higher concentrations were also observed for (+)-(S)-N-desmethyl zopiclone and (+)-(S)-N-oxide zopiclone, confirming the stereoselective disposition of zopiclone. 相似文献
19.
S. Tatar Ulu 《Chromatographia》2006,64(7-8):447-451
A simple, selective, precise and accurate reversed phase-HPLC assay for analysis of gemfibrozil in tablets was developed and validated. Separation and quantification were achieved on a Phenomenex C18 column under isocratic conditions using a mobile phase (methanol:water, 80:20, v/v) maintained at 1.1 mL min−1. UV-detection was at 280 nm. Atorvastatin was selected as an internal standard. The standard curves were linear over the range of 0.5–3.0 μg mL−1 (r > 0.999). The limits of detection and quantification were 0.20 and 0.51 μg mL−1, respectively. The recoveries for gemfibrozil were above 99.01%. The intra-day and inter-day precision (RSD) for gemfibrozil were below 1.74 and 1.83%, respectively. No chromatographic interferences from the tablet excipients were found. The results of the developed procedure in tablets were compared with those of the reference method to assess gemfibrozil content. Statistical comparison of the results with the reference method using spectrofluorimetric method showed excellent agreement and proved no significant difference in accuracy and precision. This HPLC method is fast and simple for the analysis of gemfibrozil in pharmaceutical preparations. 相似文献
20.
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