共查询到20条相似文献,搜索用时 31 毫秒
1.
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
2.
A high performance liquid chromatographic method was developed and validated for the quantitative determination of carbamazepine
in intravenous nanoemulsions. The method validation yielded good results with respect to linearity, specificity, precision
and accuracy. The method was carried out on a RP-18 column with a mobile phase composed of methanol–water (70:30 v/v) subjected to a gradient of acetonitrile after drug elution, and detection at 286 nm. The linearity in the range of 10.0–50.0 μg mL−1 presented a determination coefficient (r
2) of 0.9996, calculated by least-squares regression; the RSD values for intra-day and inter-day precision for % recovered
were <0.44 and <1.21%, respectively; and the recovery of carbamazepine from the sample matrix ranged from 94.3 to 104.9%. 相似文献
3.
Rahul P. Dixit Chandrashekhar R. Barhate Mangal S. Nagarsenker 《Chromatographia》2008,67(1-2):101-107
Simvastatin and ezetimibe are used to treat hyperlipidemia. A simple, selective and stability-indicating HPTLC method has
been established for analysis of simvastatin and ezetimibe. The method has been validated so that both drugs can routinely
be analyzed simultaneously. The method uses aluminum-backed silica gel 60F254 TLC plates as stationary phase with n-hexane–acetone 6:4 (v/v) as mobile phase. Densitometric analysis of both drugs was carried out in absorbance mode at 234 nm. This system was found
to give compact bands for simvastatin and ezetimibe (R
F 0.39 ± 0.05 and 0.50 ± 0.05, respectively). Linear relationships were obtained between response and amount of drug in the
range 200–1,600 ng per band with high correlation coefficients (r
2 = 0.9917 ± 0.0018 for simvastatin and r
2 = 0.9927 ± 0.0021 for ezetimibe). The method was validated for precision, robustness, and recovery. The limits of detection
and quantitation were 25 and 150 ng per band, respectively. Simvastatin and ezetimibe were subjected degradation by acid,
pH 6.8 phosphate buffer, oxidation, dry heat, and wet heat. The degradation products were well resolved from the pure drug
with significantly different R
F values. Because the method could effectively separate the drug from its degradation products, it can be used for stability-indicating
analysis. 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.
S. Tatar Ulu 《Chromatographia》2006,64(3-4):169-173
A new, simple, rapid and specific reversed-phase high-performance liquid chromatography (HPLC) method was developed and validated for the determination of fluvoxamine in pharmaceutical dosage forms. The HPLC separation was achieved on a C18 μ-Bondapack column (250 mm × 4.6 mm) using a mobile phase of acetonitrile–water (80:20, v/v) at a flow rate of 1 mL min−1. Proposed method is based on the derivatization of fluvoxamine with 1,2-naphthoquinone-4-sulphonic acid sodium salt (NQS) in borate buffer of pH 8.5 to yield a orange product. The HPLC method is based on measurement of the derivatized product using UV-visible absorbance detection at 450 nm. The method was validated for specificity, linearity, precision, accuracy, robustness. The degree of linearity of the calibration curves, the percent recoveries of fluvoxamine, the limit of detection and quantification, for the HPLC method were determined. The assay was linear over the concentration range of 45–145 ng mL−1 (r = 0.9999). Limit of detection and quantification for fluvoxamine were 15 and 50 ng mL−1, respectively. The results of the developed procedure (proposed method) for fluvoxamine content in tablets were compared with those by the official method. The method was found to be simple, specific, precise, accurate, reproducible and robust. 相似文献
6.
Artem U. Kulikov 《Chromatographia》2007,66(5-6):303-309
A simple micellar liquid chromatographic technique for deltamethrin determination was developed and validated. The method
provided to be suitable for deltamethrin determination in pediculicide shampoo. Kromasil C18 column (150 mm×4.6 mm, 5 μm)
and mobile phase −0.12 M sodium dodecyl sulfate with 9% (v/v) 1-butanol were used for deltamethrin separation. Detection wavelength was 265 nm. The retention time was about 15 min. Different
validation parameters were evaluated. The specificity of the method was demonstrated. Linearity was established in the range
10–40 μg L−1. The limits of detection and quantitation were 1.06 and 3.22 μg mL−1, respectively. The method showed excellent accuracy (100.6%) and precision (repeatability) gave a relative standard deviation
of less than 1%. The influence of the various method parameters (robustness study) was also studied. 相似文献
7.
A new, simple high-performance thin-layer chromatographic method has been established and validated for simultaneous determination
of escitalopram oxalate and clonazepam in a combined tablet dosage form. The drugs were separated on aluminum plates precoated
with silica gel 60 F254; toluene–ethyl acetate–triethylamine 7:3.5:3 (v/v) was used as mobile phase. Quantitative analysis was performed by densitometric scanning at 258 nm. The method was validated
for linearity, accuracy, precision, and robustness. The calibration plot was linear over the ranges 250–2,500 and 50–500 ng band−1 for escitalopram oxalate and clonazepam, respectively. The method was successfully applied to the analysis of drugs in a
pharmaceutical formulation. 相似文献
8.
Hellen Karine Stulzer Monika Piazzon Tagliari Gislaine Kuminek Paulo Renato Oliveira Charise Dallazen Bertol Marcos Antonio Segatto Silva 《Chromatographia》2009,69(Z2):123-128
An accurate, simple, reproducible, and sensitive liquid chromatographic method was developed and validated for the captopril
determination in controlled release tablets. The analyses were performed at room temperature on a reversed-phase Phenomenex
Luna C18 column (250 mm × 4.6 mm). The mobile phase was composed of water:methanol (45:55; v/v) pH 2.5, and it was eluted isocratically at a 1.0 mL min−1 flow rate. The method was validated in terms of specificity, linearity, quantification limit, detection limit, accuracy,
precision and robustness. The response was linear in the range 0.3–1.5 mg mL−1 (r
2
= 0.9983). The relative standard deviation values for inter-and intra-day precision were 0.77% and 0.50%, respectively. Recoveries
ranged between 97.7 and 99.1%. The method was successfully applied for the determination of captopril in the developed formulations. 相似文献
9.
M. J. e. Souza D. R. Nogueira L. M. Silva M. Z. Arend P. S. Souza Filho A. M. Bergold 《Chromatographia》2007,65(7-8):401-406
An isocratic high-performance liquid chromatographic method has been developed for assay of ceftiofur sodium in drug substance
and in sterile powder for injection. Chromatography was performed on a 250 mm × 4.6 mm, 5 μm particle, C18 column with a 78:22 (v/v) mixture of 0.02 m disodium hydrogen phosphate buffer (pH adjusted to 6.0 with 85% orthophosphoric acid) and acetonitrile as mobile phase, at
a flow rate of 1.0 mL min−1. The separation was monitored by UV detection at 292 nm. Validation of the method for linearity and range, intra- and inter-day
precision, accuracy, specificity, recovery, robustness, and limits of quantification and detection yielded good results. The
calibration plot was linear from 20.0–120.0 μg mL−1 and the correlation coefficient was 0.9999. It was shown that ceftiofur was degraded under acidic, alkaline, oxidative, and
photolytic conditions. The method was found to be stability-indicating and could be used for routine analysis of ceftiofur
sodium for injection. 相似文献
10.
Ning Ma Wen-Ying Liu Huan-De Li Xin-Yu Jiang Bi-Kui Zhang Rong-Hua Zhu Feng Wang Wei Liu Xia Liu Da-Xiong Xiang 《Chromatographia》2007,66(3-4):251-255
(E)-3,5,4′-trimethoxystilbene (BTM-0512) is a resveratrol analog with a variety of pharmacological action, including anti-cancer
properties, anti-allergic activity, estrogenic activity, antiangiogenic activity, and vascular-targeting activity against
microtubule-destabilization. There is, however, no validated analytical method for quantification of (E)-3,5,4′-trimethoxystilbene in biological matrices, so pharmacokinetic data and suitable methods for determination of the
compound in plasma are currently lacking. A rapid and sensitive liquid chromatographic–mass spectrometric method for determination
of (E)-3,5,4′-trimethoxystilbene in rat plasma, using carbamazepine as internal standard, has been developed and validated. Plasma
samples were treated with acetonitrile to precipitate proteins. Samples were then analyzed by HPLC on a 250mm × 4.6 mm i.d.,
5-μm particle, C18 column with methanol–water, 80:20 (v/v), containing 10 mm ammonium acetate and 0.2% formic acid (pH 3.0), as mobile phase, delivered at 0.85 mL min−1. A single-quadrupole mass spectrometer with an electrospray interface operated in selected-ion monitoring mode was used to
detect [M + H]+ ions at m/z 271.3 for (E)-3,5,4′-trimethoxystilbene and m/z 237.5 for the internal standard. (E)-3,5,4′-trimethoxystilbene and the internal standard eluted as sharp, symmetrical peaks with retention times of 8.9 and 4 min,
respectively. Calibration plots for (E)-3,5,4′-trimethoxystilbene in rat plasma at concentrations ranging from 0.01 to 5.0 μg mL−1 were highly linear. Intra-day and inter-day precision, as RSD, was <12.9%, and accuracy was in the range 94.8–104.7%. The
limit of detection in plasma was 0.005 μg mL−1. The method was successfully used to determine the concentration of (E)-3,5,4′-trimethoxystilbene after oral administration of 86 mg kg−1 of the drug to Sprague–Dawley rats and can be used to investigate the pharmacokinetics of the compound. 相似文献
11.
A. Önal 《Chromatographia》2006,64(7-8):459-461
A reversed-phase high-performance liquid chromatographic (HPLC) method with UV detection was developed and validated for the determination of ropinirole (ROP) in tablets. The assay utilized UV detection at 250 nm and a Luna CN column (250 × 4.6 mm I.D, 5 μm). The mobile phases were comprised of acetonitrile: 10 mM nitric acid (pH 3.0) (75:25, v/v). Validation experiments were performed to demonstrate linearity, accuracy, precision, limit of quantitation (LOQ), limit of detection (LOD), and robustness. The method was linear over the concentration range of 0.5–10.0 μg mL−1. The method showed good recoveries (99.75–100.20%) and the relative standard deviations of intra and inter-day assays were 0.38–1.69 and 0.45–1.95%, respectively. The method can be used for quality control assay of ropinirole. 相似文献
12.
A simple, rapid and reproducible HPLC method was developed and validated for the simultaneous determination of olmesartan
(OLM) medoxomil and hydrochlorothiazide (HCT) in combined tablets. Chromatography was carried out on a 4.6 mm I.D × 200 mm,
5 μm cyano column with methanol–10 mM phosphoric acid containing 0.1% triethylamine (pH 2.5, 50:50 v/v) at a flow rate of 1.0 mL min−1 and UV detector was set at 260 nm. Valsartan (VAL) was used as internal standard (IS). A linear response was observed in the
range of 0.2–6 μg mL−1 (r
2 = 0.9998) for OLM and 0.1–4 μg mL−1 (r
2 = 0.9999) for HCT, respectively. The method showed good recoveries (99.56% for OLM and 99.48% for HCT) and the relative standard
deviation (RSD) values for intra- and inter-day precision were 0.70–1.59 and 0.80–2.00% for OLM and 1.20–1.37 and 1.63–1.93%
for HCT, respectively. The developed method was applied successfully for quality control assay of OLM and HCT in combined
tablets and in vitro dissolution studies. 相似文献
13.
Stability-Indicating LC Determination of Nitazoxanide in Bulk Drug and in Pharmaceutical Dosage Form
Vipul P. Rane Jaiprakash N. Sangshetti Kiran R. Patil Ravindra D. Yeole Devanand B. Shinde 《Chromatographia》2008,67(5-6):455-459
A novel stability-indicating high-performance liquid chromatographic assay method was developed and validated for quantitative
determination of nitazoxanide in bulk drugs and in pharmaceutical dosage form in the presence of degradation products generated
from forced decomposition studies. An isocratic, reversed phase LC method was developed to separate the drug from the degradation
products, using an Ace5- C18 (250 mm × 4.6 mm, 5 μm) column, and 50 mM ammonium acetate (pH 5.5 by acetic acid) and acetonitrile
(55:45 v/v) as a mobile phase. The detection was carried out at a wavelength of 240 nm. The nitazoxanide was subjected to stress conditions
of hydrolysis (acid, base), oxidation, photolysis and thermal degradation. Degradation was observed for nitazoxanide in base,
acid and in 30% H2O2 conditions. The drug was found to be stable in the other stress conditions attempted. The degradation products were well
resolved from the main peak. The percentage recovery of nitazoxanide was from (100.55 to 101.25%) in the pharmaceutical dosage
form. The developed method was validated with respect to linearity, accuracy (recovery), precision, system suitability, specificity
and robustness. The forced degradation studies prove the stability indicating power of the method. 相似文献
14.
A stability-indicating HPLC assay method was developed for the quantitative determination of tadalafil in bulk samples and
in pharmaceutical dosage forms in the presence of the degradation products. It involved a 250 mm × 4.6 mm, 5 μm C-18 column.
The gradient LC method employs solution A and B as mobile phase. Solution A contains a mixture of buffer (phosphate buffer
and tetra-n-butyl ammonium hydrogen sulfate) pH 2.5: acetonitrile (80:20, v/v) and solution B contains a mixture of water: acetonitrile (20:80, v/v). The flow rate was 1.0 mL min−1 and the detection wavelength was 220 nm. The retention time of tadalafil is about 17 min. Tadalafil was subjected to different
ICH prescribed stress conditions. Degradation was found to occur in hydrolytic and to some extent in oxidative stress conditions,
while the drug was stable to photolytic and thermal stress. The drug was particularly labile under alkaline hydrolytic conditions.
The drug was subjected to stress conditions of hydrolysis, oxidation, photolysis and thermal degradation. The assay of stress
samples was calculated against a qualified reference standard and the mass balance was close to 99.5%. The developed RP-LC
method was validated with respect to linearity, accuracy, precision and ruggedness. 相似文献
15.
Danieli Cátia Ceni Laura Alegria Martins Andréa Garcia Pereira Pedro Eduardo Fr?ehlich Ana Maria Bergold 《Chromatographia》2009,69(Z2):189-194
A reversed-phase ion-pairing liquid chromatographic method was developed and validated for the assay of Fe(II) in ferrous
bisglycinate (Fe-bis-gly) capsules using 4-(2-pyridylazo) resorcinol reagent. The analysis was carried out using a Gemini
RP-18 (150 mm × 4.6 mm I.D., particle size 5 μm) analytical column; the mobile phase consisted of a mixture of acetonitrile–water
(28:72 v/v) containing 1 mM tetrabutylammonium hydrogensulfate and 1% phosphate buffer (pH 8.0). The flow rate was 1.0 mL min−1 and the detection was achieved with a photodiode array (PDA) detector at 706 nm. The specificity of the method was proved
using stress conditions and evaluated using a PDA detector. The data validation showed that the method is specific, fast,
accurate, and reproducible for the determination of Fe-bis-gly in dosage form. The response was linear over a range of 1.0–2.6 μg mL−1 (r = 0.9999). The accuracy of the method ranged from 98.02 to 102.75%. The RSD values for intra- and inter-day precision studies
were below 1.3 and 1.1%, respectively. There was no interference of the excipients on the determination of the active pharmaceutical
ingredient. 相似文献
16.
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
17.
Uttam Mandal Amlan Kanti Sarkar Kadagi Veeran Gowda Sangita Agarwal Anirbandeep Bose Uttam Bhaumik Debotri Ghosh Tapan Kumar Pal 《Chromatographia》2008,67(3-4):237-243
A bioanalytical method has been developed and validated for determination of pregabalin in human plasma. The analytical method
consists in the precipitation of plasma sample with trichloro acetic acid (20% v/v solution in water), followed by the determination of pregabalin by an LC-MS-MS method using gabapentin as internal standard.
Separation was achieved on a Gemini C18 50 mm × 2.0 mm (3 μm) column with an isocratic mobile phase consisting of methanol–water (98:2, v/v) with 0.5% v/v formic acid. Protonated ions formed by a turbo ionspray in positive mode were used to detect analyte and internal standard.
The MS-MS detection was by monitoring the fragmentation of 160.2→55.1 (m/z) for pregabalin and 172.2→67.1 (m/z) for gabapentin on a triple quadrupole mass spectrometer. The assay was calibrated over the range 0.1–15.0 μg mL−1 with correlation coefficient of 0.9998. Validation data showed intra-batch (n = 6) CV% ≤ 6.89 and RE (%) between −4.17 and +3.08 and inter-batch (n = 18) CV% < 9.09 and RE (%) between −3.0 and +10.00. Mean extraction recovery were 80.45–89.12% for three QC samples and 87.56%
for IS. Plasma samples were stable for three freeze–thaw cycles, or 24 h ambient storage, or 1 and 3 months storage at −20 °C.
Processed sample (ready for injection) were stable up to 72 h at autosampler (4 °C). This method has been used for analyzing
plasma samples from a bioequivalence study with 18 volunteers. 相似文献
18.
Marcelo Donadel Malesuik Simone Gonçalves Cardoso Martin Steppe 《Chromatographia》2008,67(1-2):131-136
A reversed-phase liquid chromatographic (LC) method was developed for the assay of nitazoxanide (NTZ) in solid dosage formulations.
An isocratic LC separation was performed on a Phenomenex Synergi Fusion C18 column (250 mm × 4.6 mm, i.d., 4 μm particle size) using a mobile phase of 0.1% o-phosphoric acid solution, pH 6.0: acetonitrile (45:55, v/v) at a flow rate of 1.0 mL min−1. Detection was achieved with a photodiode array detector at 240 nm. The detector response for NTZ was linear over the concentration
range from 2 to 100 μg mL−1 (r = 0.9999). The specificity and stability-indicating capability of the method were proved using stress conditions. The RSD
values for intra-day precision were less than 1.0% for tablets and powder for oral suspension. The RSD values for inter-day
precision were 0.6 and 0.7% for tablets and powder for oral suspension. The accuracy was 100.4% (RSD = 1.8%) for tablets and
100.9% (RSD = 0.3%) for powder for oral suspension. The limits of quantitation and detection were 0.4 and 0.1 μg mL−1. There was no interference of the excipients on the determination of the active pharmaceutical ingredient. The proposed method
was precise, accurate, specific, and sensitive. It can be applied to the quantitative determination of drug in tablets and
powder for oral suspension. 相似文献
19.
Spyros Drivelos Marilena E. Dasenaki Nikolaos S. Thomaidis 《Analytical and bioanalytical chemistry》2010,397(6):2199-2210
A new hydrophilic interaction liquid chromatographic (HILIC) method for the simultaneous determination of isoascorbic (IAA)
and ascorbic acid (AA) was developed. The separation of IAA and AA was studied in various HILIC stationary phases and the
influence of the composition of the mobile phase, the ionic strength and the column temperature to the chromatographic characteristics
is presented. The final method used an aminopropyl column under isocratic elution with acetonitrile–100 mM ammonium acetate
solution (90:10, v/v) at a flow rate of 0.4 mL/min and a detection wavelength of 240 nm. This method was validated and the calibration curves
were found to be linear in the range of 1.0–65 μg/mL for both IAA and AA. The method limit of detection for IAA determination
in fish tissue was 2.3 μg/g. Inter-day precision (as %RSDR) was ranged between 0.56% and 8.3% at three concentration levels, whereas the respected recoveries ranged between 82% and
98%. This method was applied to the determination of IAA (as additive E315) in frozen redfish samples. The hyphenation of
the HILIC separation with a tandem mass spectrometer was also studied and the problems encountered with negative electrospray
ionization under HILIC separation conditions are discussed. 相似文献
20.
A stability-indicating reversed-phase liquid chromatographic (RPLC) method has been established for analysis of ramipril (RAM)
and moexipril hydrochloride (MOEX.HCl) in the presence of the degradation products generated in studies of forced decomposition.
The drug substances were subjected to stress by hydrolysis (0.1 m NaOH and 0.1 m HCl), oxidation (30% H2O2), photolysis (254 nm), and thermal treatment (80 °C). The drugs were degraded under basic and acidic conditions and by thermal
treatment but were stable under other stress conditions investigated. Successful separation of the drugs from the degradation
products was achieved on a cyanopropyl column with 40:60 (v/v) aqueous 0.01 m ammonium acetate buffer (pH 6)–methanol as mobile phase at a flow rate of 1 mL min−1. Detection was by UV absorption at 210 nm. Response was a linear function of concentration over the range 5–50 μg mL−1 (r > 0.9995), with limits of detection and quantitation (LOD and LOQ) of 0.04 and 0.09 μg mL−1, respectively, for RAM and 0.014 and 0.32 μg mL−1, respectively, for moexipril. The method was validated for specificity, selectivity, solution stability, accuracy, and precision.
Statistical analysis proved the method enabled reproducible and selective quantification of RAM and MOEX as the bulk drug
and in pharmaceutical preparations. Because the method effectively separates the drugs from their degradation products, it
can be used as stability-indicating. 相似文献