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1.
Two validated analytical methods have been developed to determine glimepiride in pharmaceutical formulations using HPLC and
1st order derivative spectrophotometric techniques. Employing reverse phase HPLC method, the drug was analyzed by pumping
a mixture of acetonitrile and 2% formic acid solution, pH 3.5 (80: 20 v/v) through a C18 column (250 × 4.6 mm, 5 μm) and detecting the eluents at 228 nm. The linearity range was found to be 20–140 μg/mL with mean
recovery of 100.52 ± 0.33%. The second method was based on the formation of a complex of the drug with 2,3,5-triphenyl-2H-tetrazolium
chloride in basic media. 1st order derivative spectrum made it possible to detect the complex at 413.5 nm. The linearity range
was found to be 40–160 μg/mL, with mean recovery of 100.33 ± 0.47%. Both the proposed methods can reliably be used for routine
analysis of glimepiride in raw material as well as in pharmaceutical formulations.
The article is published in the original. 相似文献
2.
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
3.
Facile LC‐UV methods for simultaneous monitoring of ciprofloxacin and rosuvastatin in API,formulations and human serum 下载免费PDF全文
An efficient, selective and cost‐effective liquid chromatographic assay was developed and validated for the simultaneous quantification of ciprofloxacin and rosuvastatin in Active Pharmaceutical Ingredients (API), pharmaceutical formulations and in human serum. The chromatographic system consisted of mobile phase methanol–water, 90:10 v/v at pH 3.0 adjusted with o‐phosphoric acid, pumped at 1.0 mL/min through a prepacked Purospher Star C18 (5 µm, 25 × 0.46 cm) column and effluent was monitored at the isosbestic point (255 nm) as well as at the λmax of individual drugs (243 and 271 nm). The method was validated over a linear concentration range of 0.25–15 µg/mL for ciprofloxacin and 0.33–20 µg/mL for rosuvastatin (r2 ≥ 0.999). The ranges of reliable response (limits of detection and quantitation) for ciprofloxacin were 3–15 and 9–45 ng/mL and 17–29 and 52–88 ng/mL, respectively, for rosuvastatin in all API, pharmaceutical formulations and human serum. Analytical recovery from human serum was >98% and relative standard deviation (RSD) was <2. The accuracies were 97.13–102.55 and 97.41–101.31% and precisions in RSD were 0.04–1.90 and 0.02–1.23% for ciprofloxacin and rosuvastatin, respectively. No matrix interferences, ion suppression/enhancement and carry‐over were detected. The total assay run time was less than 5 min. In another study, for optimum performance the detector was programmed for multiwavelength scanning at the absorption maxima of each component. Consequently, the linearity range was improved and limit of detection and quantitation values were down to 1–4 and 4–12 ng/mL for ciprofloxacin and 3–5 and 9–15 ng/mL for rosuvastatin, respectively. The validation parameters fitted ICH guidelines through the isosbestic and individual λmax approach. The small sample volume and simplicity of preparation make this method suitable for use in human serum samples, pharmaceutical formulations, quality control, drug–drug interaction studies, clinical laboratories, drug research centers and forensic medical centers. Copyright © 2014 John Wiley & Sons, Ltd. 相似文献
4.
M. A. Naushad M. Aqil F. J. Ahmad A. Ali M. S. Faisal M. Rizwan S. Faiyaz 《Journal of Analytical Chemistry》2008,63(10):965-970
A simple, economic, selective, precise, and accurate high-performance liquid chromatographic (HPLC) method for the analysis of trimetazidine hydrochloride in both bulk drug and pharmaceutical formulations was developed and
validated in the present study. The mobile phase consisted of water: methanol: triethylamine (75: 25: 0.1 v/v/v), and pH 3.3
was adjusted with orthophosphoric acid. This system was found to give a sharp peak of trimetazidine hydrochloride at a retention
time of 3.375 ± 0.04 min. HPLC analysis of trimetazidine hydrochloride was carried out at a wavelength of 232 nm with a flow
rate of 1.0 mL/min. The linear regression analysis data for the calibration curve showed a good linear relationship with a
regression coefficient of 0.997 in the concentration range of 5–90 μg/mL. The linear regression equation was y = 35362x −
8964.2. The limit of detection (LOD) and limit of quantification (LOQ) were found to be 3.6 and 10.9 μg/mL, respectively. The developed method was employed with a high degree of precision and
accuracy for the analysis of trimetazidine hydrochloride. The developed method was validated for accuracy, precision, robustness,
detection, and quantification limits as per the ICH guidelines. The wide linearity range, accuracy, sensitivity, short retention
time, and composition of the mobile phase indicated that this method is better for the quantification of trimetazidine hydrochloride.
The text was submitted by the authors in English. 相似文献
5.
A simple, economical, and automated spectrophotometric method for the determination of chlorpromazine hydrochloride by sequential
injection analysis using ammonium metavanadate as colorimetric reagent is proposed. The various chemical and physical conditions
that affected the reaction have been thoroughly investigated. The calibration curve was linear within the range 10–100 μg/mL.
The detection limit (S/N = 3) was 0.7 μg/mL and the limit of quantification (S/N = 10) was 2.3 μg/mL. The sampling frequency was 22 h−1. The method has been used for the determination of chlorpromazine hydrochloride in pure form and pharmaceutical formulations.
The t-test has revealed that there is no evidence of significant differences between the obtained results at the 95% confidence
level. The method can be applied to the quantitative determination of chlorpromazine hydrochloride. It is also applicable
in the quality control of chlorpromazine hydrochloride preparations.
The text was submitted by the authors in English. 相似文献
6.
Al-Hamdi AM Williams JR Al-Kindy SM Pillay AE 《Applied biochemistry and biotechnology》2006,135(3):209-218
A rapid reversed-phase (RP) high-performance liquid chromatography method for the isolation of bilirubin from its photoproducts
(e.g., biliverdin) is reported. The method is based on isocratic elution using methanol:water as the mobile phase. A 24 full-factorial experimental design approach was adopted. For the optimization, the best separation was obtained using a flow
rate of 1.50 mL/min, a mobile phase of 99∶1 methanol:water (v/v) at pH 3.60, and a 150×4.6 mm id RP (C18) column containing 5-μm particles. These conditions produced the fastest total retention time of 3.38±0.055 min, and other
chromatographic parameters were acceptable. Under the optimum conditions, a linear calibration curve for bilirubin was obtained
over the 1.0–40.0 μg/L concentration range studied. The limit of quantification was 0.79 g/L and the limit of detection was
0.24 μg/L. Bilirubin in solution was monitored by ultraviolet detection at 450 nm. 相似文献
7.
B. S. Nagaralli J. Seetharamappa B. G. Gowda M. B. Melwanki 《Journal of Analytical Chemistry》2003,58(8):778-780
A simple, rapid, and precise high-performance liquid chromatographic method for the determination of nimesulide in pharmaceutical preparations was proposed using Ibuprofen as an internal standard. The separation was performed on a CLC C18 (5 m, 25 cm × 4.6 mm i.d.) column with a mobile phase consisting of an acetonitrile–0.05 M KH2PO4 buffer mixture of pH 7.00 (55 : 45, v/v). The detection was carried out at 230 nm and the linearity range was found to be 0.5–100 g/mL. The method has been applied successfully to the determination of nimesulide in pharmaceutical formulations. The recovery values were found to be in the range of 99.23–100.13% with RSD values of less than 0.97%. 相似文献
8.
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
9.
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
10.
A simple, reproducible, and sensitive extraction-spectrophotometric method for the determination of fluoxetine (FL) in pharmaceutical formulations is reported. The FLH+ cation, which is formed in an acidic solution, can form an ion-pair with Orange II, (OR II), an anionic dye. The FLH+-OR II− ion pair was quantitatively extracted into dichloromethane solvent and its absorption was measured at 482 nm. The calibration
graph is linear over the FL concentration range of 0.2–9.0 μg/mL and the regression coefficient is 0.9995. The relative standard
deviation (RSD) of ten replicate determinations of 5.0 and 1.4 μg/mL of FL are 0.022 and 0.038, respectively, and the limit
of detection (LOD) of the method is 0.17 μg/mL. The method was successfully applied to the determination of an FL amount in
pharmaceutical formulations (10.0-and 20.0-mg capsules).
The text was submitted by the authors in English. 相似文献
11.
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
12.
R. Zakrzewski 《Journal of Analytical Chemistry》2009,64(12):1235-1241
A high-performance liquid chromatographic method of reversed-phase with a post-column iodineazide reaction has been developed
and validated for the determination of thioguanine. Isocratic elution was performed on a column of C18 using acetonitrile- water-sodium azide solution (1.5%; pH 6.5) 16: 34: 50 (v/v/v) as a mobile phase with flow-rate of 0.5
mL/min. Monitoring of unreacted iodine in post-column iodine-azide reaction induced by thioguanine resulted in its detection
at 350 nm. The method applied to thioguanine was linear within the scope of values 8–100 nM (r
2 > 0.9988). The relative standard deviation (RSD < 4.2%) and the recovery (>96%) prove that the intra-day precision and the
accuracy were satisfactory. The lower limits of detection (LLD) and quantification (LLQ) of thioguanine were established at the levels of 6 and 8 nM, respectively. The elaborated method was validated and applied
to thioguanine determination in tablets. 相似文献
13.
Development and validation of a generic liquid chromatographic method for the simultaneous determination of five commonly used antimalarial drugs: Application to pharmaceutical formulations and human plasma 下载免费PDF全文
Sai Sandeep Mannemala Janaki Sankarachari Krishnan Nagarajan 《Journal of separation science》2015,38(9):1521-1528
A simple, sensitive, and rapid liquid chromatographic method was developed and validated using diode array detection for the determination of five commonly used antimalarial drugs in pharmaceutical formulations and in human plasma. Chromatographic separation of antimalarial drugs and internal standard (ibuprofen) was achieved on a C18 column with a mobile phase composed of 10 mM dipotassium orthophosphate at pH 3.0, methanol, and acetonitrile in a ratio of 20:38:42 v/v, at a flow rate of 1 mL/min. The analytes were monitored at 220 nm and separated in ?10 min. The method was validated for linearity, accuracy, precision, limit of quantification, and robustness. Both intra‐ and interday precisions (in terms of %RSD) were lower than 3% and accuracy ranged from 98.1 to 104.5%. Extraction recoveries were ≥96% in plasma. The limits of quantitation for artemether, lumefantrine, pyrimethamine, sulfadoxine, and mefloquine were 0.3, 0.03, 0.06, 0.15, and 0.15 μg/mL in human plasma. Stability under various conditions was also investigated. The method was successfully applied for quantification of antimalarial drugs in marketed formulations and in spiked human plasma. The method can be employed for routine QC purposes and in pharmacokinetic investigations. 相似文献
14.
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
15.
Summary A sensitive and rapid routine HPLC method is proposed for quantitative estimation of morphine hydrochloride and hydromorphone
hydrochloride in pharmaceutical dosage forms. The drugs were chromatographed on a C18 reversed-phase column; the mobile phase was acetonitrile-water, 35:65 (v/v), containing sodium dodecyl sulphate (0.5%, w/v),
as ion pairing reagent, and acetic acid (0.4% v/v). Detection was at 230 nm.
The optimized method was validated and linearity (r>0.999), precision, and accuracy were found to be acceptable within the concentration ranges 86–124 μg mL−1 for morphine hydroloride and 60–180 μg mL−1 for hydromorphone hydrochloride.
The method is being used to investigate the stability of morphine hydrochloride and hydromorphone hydrochloride in solution
used for intramuscular injection. 相似文献
16.
I. V. Semak N. A. Alekseev E. O. Korik A. M. Drobyshevskii M. V. Antonova 《Journal of Analytical Chemistry》2011,66(2):195-200
A procedure has been developed for the determination of a macrolide antibiotic roxythromycin (RX) in blood serum using HPLC
with mass spectrometric detection using clarithromycin (CL) as the internal standard. RX and CL have been extracted from the
samples by solid-phase extraction in a cartridge filled with a polar adsorbent, cyanopropylsilyl silica gel. The absolute
recoveries of RX and CL are 89.6 and 92.5%, respectively. Chromatographic separation has been performed on a Nucleodur C18 Isis column with the mobile phase composed as follows: water-methanol-acetonitrile-formic aid (499: 250: 250: 1 by volume).
Registration has been performed in the mode of selected ion monitoring with m/z 837.7 (RX) and m/z 748.7 (CL). The analytical range for RX is 0.097–14.81 μg/mL, the quantification limit is 0.097 μg/mL, the detection limit
is 0.03 μg/mL, and the intraday and interday relative standard deviation are 2–6 and 4–8% respectively. The procedure has
been applied to the pharmacokinetic studies of the Rulid pharmaceutical preparation. 相似文献
17.
G. S. Nikoli? I. Savi? V. Marinkovi? 《Russian Journal of Physical Chemistry A, Focus on Chemistry》2009,83(9):1609-1611
A selective, precise and new high-performance liquid chromatographic method for the analysis of loperamid hydrochloride in
pharmaceutical formulations was developed and validated. The mobile phase consisting buffer (sodium-octansulphonate, triethylamine
and ammonium hydroxide) in water: acetonitriie (45: 55, v/v) (pH 3.2). The absorbance was monitored with a DAD detector at
226 nm. The flow rate was 1.5 cm3 min−1. The linearity (r = 0.9947) and the recovery (98.58–100.42%) were found to be satisfactory. The detection and quantitation limits were found
to be 0.95 and 3.12 μg cm−3. The results demonstrated that the procedure was accurate, precise and reproducible. It can be suitably applied for the estimation
of lopera-mid hydrochloride in pharmaceutical formulations.
The article is published in the original. 相似文献
18.
A. Phonchai B. Janchawee S. Prutipanlai S. Thainchaiwattana 《Journal of Analytical Chemistry》2010,65(9):951-959
A methodology for the determination of 3,4-methylenedioxymethamphetamine (MDMA), 3,4-methylenedioxyamphetamine (MDA) and methamphetamine (MA) in seized tablets using gas chromatography with a flame ionization detector (GC-FID) is described. The chromatographic conditions, i.e. gas flow rates and temperatures for the column, injector and detector
were optimized. The optimum chromatographic conditions were as follows: a CP-SIL 24 CB WCOT fused silica capillary column
(30 m × 0.32 mm I.D., 0.25 μm film thickness), N2 carrier gas flowing at 2.6 mL/min, injector temperature at 290°C and detector temperature at 300°C. The oven temperature
was ramped from 80°C at a rate of 20°C/min to final temperature of 270°C (1 min). All analytes were well separated within
7 min with an analysis time of 10.5 min. Calibration curves were linear over the concentration ranges of 3.125–200 μg/mL for
MDMA and 6.25–200 μg/mL for MDA and MA (r > 0.990). The intra- and inter-day precisions for determining all analytes were 2.32–10.38% RSD and 1.15–9.77% RSD, respectively.
The intra- and inter-day accuracies ranged from −19.79 to +17.51% DEV and −6.84 to +5.2% DEV, respectively. The lower limits
of quantification (LLOQs) were 3.125 μg/mL for MDMA and 6.25 μg/mL for MDA and MA. All analytes were stable at room temperature during 24 h but significant
loss occurred after 2-month storage at −20°C. The method was shown to be useful for determining the purity of MDMA in seized
tablets. 相似文献
19.
López-Flores J Fernández-de Córdova ML Molina-Díaz A 《Analytical and bioanalytical chemistry》2007,388(8):1771-1777
A flow injection–solid-phase spectroscopy (FI-SPS) system implemented with photochemically induced fluorescence (PIF) is described
for the rapid and very sensitive determination of reserpine in biological fluids and pharmaceutical formulations. An intensively
fluorescent photoproduct is in-line generated, retained on C18 silica gel in the detection area and monitored at 394/489 nm (λ
ex/λ
em). After the establishment of the appropriate working variables, the system is calibrated at two different injection volumes,
100 and 800 μL, achieving detection limits of 0.33 and 0.05 ng mL−1, respectively. The RSD for reserpine at 2 ng mL−1 (800 μL) was 1.5% (n = 10). The sampling rates were 46 and 43 h−1 for each injection volume, respectively. The potential interference of some common species coexisting with reserpine in the
analysed samples was also studied. The procedure was successfully applied to commercial formulations, urine and serum without
any previous treatment of samples. Recoveries ranged from 94.9 to 100.2%. 相似文献
20.
Two simple, rapid and reproducible spectrophotometric methods have been described for the assay of olmesartan (OLM) in pharmaceutical formulation. The methods are based on the formation of ion associates in the reactions between the studied
drug substance and ion-pair agents [bromocresol green (BCG) and bromophenol blue (BPB)]. By the extraction with dichloromethane and chloroform, yellow-colored ion associates were formed in acidic medium and
absorbances were measured at 409 (BCG) and 412 nm (BPB). Optimizations of the reaction conditions were performed. Beer’s law
was obeyed within the concentration range from 1–40 μg/mL and 10–120 μg/mL, respectively, for BCG and BPB. The molar absorptivity,
detection and quantification limits were also determined. The developed methods were applied successfully to the determination
of this drug in tablets. 相似文献