Application of column-switching HPLC method in evaluating pharmacokinetic parameters of zaltoprofen and its salt

2009 ◽  
Vol 23 (5) ◽  
pp. 537-542 ◽  
Author(s):  
Hyun Kyoung Yang ◽  
Seo Young Kim ◽  
Joon Seop Kim ◽  
Hongkee Sah ◽  
Hwa Jeong Lee

Author(s):  
Yan Xiong ◽  
Yong-Hong Liu ◽  
Jian-Sha Li ◽  
Yu-Ying Zhang ◽  
Jing Zhang ◽  
...  

Abstract A simple high performance liquid chromatography (HPLC) method was developed and validated for the determination of coumarin-3-carboxylic acid analogues (C3AA) in rat plasma and a preliminary study on pharmacokinetics. Ferulic acid (FA) was used as the internal standard substance, and coumarin-3-carboxylic acid (C3A) was used as a substitute for quantitative C3AA. After protein precipitation with methanol, the satisfactory separation was achieved on an ODS2 column when the temperature was maintained at 30 ± 2°C. The correlation coefficient r in the C3A linear equation is equal to 0.9990. Pharmacokinetic parameters for t1/2, Tmax, Cmax, area under the curve (AUC)0-t, average residence time (MRT), apparent volume of distribution (V z/F) and clearance (Cl/F) were 1.89 ± 0.03 h, 0.39 ± 0.14 h, 1.81 ± 0.10 g· mL−1 ·h, 7.88 ± 0.24 g·mL−1·h, 3.23 ± 0.14 h, 0.43 ± 0.03 (mg·kg−1)·(g·mL−1)−1·h−1, respectively. The high performance liquid chromatography-photo diode array detector (HPLC-PDA) method established in this study can be used to separate and determine the content of C3AA in plasma of rats after 60% ethanol extraction by gavage. The plasma concentration-time curve and pharmacokinetic parameters reflect the absorption of C3AA in rat blood after oral administration to some extent.



Author(s):  
Aruna G. ◽  
Bharathi K ◽  
Kvsrg Prasad

Objective: To develop and validate a modified isocratic reversed-phase high performance liquid chromatographic (RP-HPLC) method for determination of cilnidipine and nebivolol in human plasma to be used for pharmacokinetic studies.Methods: The drug was extracted from plasma samples by direct protein precipitation technique using acetonitrile. Amlodipine was used as internal standard (IS). Samples were analyzed on BDS C18 column (250 x 4.6 mm, 5 µm), applying ortho phosphoric acid (0.1%): Acetonitrile, at a ratio of 45:55 v/v in isocratic mode as a mobile phase at a flow rate of 1 ml/min to attain adequate resolution. Separations were performed at room temperature and monitored at a wavelength of 260 nm after injection of 50μl samples into the HPLC system. The analytical method was validated according to FDA bioanalytical method validation guidance. The method was applied for pharmacokinetic study of cilnidipine and nebivolol tablets-10 mg and 5 mg were administered as a single dose to 6 healthy male rabbits under fasting condition. Twelve blood samples were withdrawn from each rabbit over 24 h periods. From the plasma concentration-time data of each individual, the pharmacokinetic parameters; Cmax, Tmax, AUC0-t and AUC0-∞ were calculated.Results: A peak area was obtained for cilnidipine and nebivolol at 3.943 and 4.719 min retention time respectively. Linearity was established at a concentration range of 0.20-20 μg/ml (r2=0.999, n=8) for cilnidipine and 0.02-2 μg/ml (r2=0.999, n=8) for nebivolol. The lower limit of quantitation (LLOQ) was identifiable and reproducible at 0.2μg/ml for cilnidipine and 0.02 μg/ml for nebivolol. The coefficients of variation (%cv) of the intra-day and inter-day precision of cilnidipine at 600, 1000 and 1600ng/ml levels were found to be 6.90%, 6.19%, 5.22%; and 7.74%, 6.54%, 5.77%, respectively, which are lower than the accepted criteria limits (15-20 %). The mean recovery (%) cilnidipine at 600, 1000, and 1600ng/ml was found to be 101.03%, 99.27% and 104.87%, and for nebivolol 60, 100, and 160 ng/ml was found to be 106.13%, 107.03% and 98.06% respectively. Stability at different conditions and in autosampler was also established. The mean pharmacokinetic parameters; Cmax, Tmax, AUC0-t and AUC0-∞ were 6 ng/ml, 2 hr, 96.76 mg. hr/ml, 63.45 mg. hr/ml for cilnidipine and 5.8ng/ml, 2hr, 74.78 mg. hr/ml, 100.25 mg. hr/ml for nebivolol respectively.Conclusion: The present analytical method was found to be specific, sensitive, accurate and precise for quantification of cilnidipine and nebivolol in human plasma. It can be successively applied for pharmacokinetics, bioavailability and bioequivalence studies.



2010 ◽  
Vol 33 (21) ◽  
pp. 3292-3298 ◽  
Author(s):  
Yumiko Akamine ◽  
Norio Yasui-Furukori ◽  
Midori Kojima ◽  
Yoshimasa Inoue ◽  
Tsukasa Uno


2021 ◽  
Vol 2021 ◽  
pp. 1-6
Author(s):  
Hua-ling Xia ◽  
Xin-jie Zhao ◽  
Yu-ji Zhang ◽  
Xiao-hang Su ◽  
Bo Sun ◽  
...  

A sensitive high-performance liquid chromatography (HPLC-UV) method for determination of omeprazole in beagle dog plasma was developed and to investigate the effect of Sijunzi pills (SJZPs) on the pharmacokinetics of omeprazole in beagle dogs. The beagle dog plasma was extracted with ethyl acetate and n-hexane under alkaline conditions. Omeprazole and internal standard (IS, fluconazole) were separated on an XDB-C18 column, and acetonitrile and 0.1% trifluoroacetic acid were used as the mobile phase. Omeprazole and IS were detected by using a diode array detector. This experiment adopts the experimental design of double-cycle self-control. In the first cycle (group A), six beagle dogs were given omeprazole 0.67 mg/kg orally in a single dose. In the second period (group B), the same six beagle dogs were orally given SJZPs 0.2 g/kg twice a day for 7 consecutive days, and then, omeprazole was orally given. At the different time points after omeprazole was given in the two periods, the blood samples were collected. The concentration of omeprazole was detected by the developed HPLC method. DAS 2.0 was used to calculate the pharmacokinetic parameters of omeprazole. Under the current experimental conditions, this UPLC method showed good linearity in the detection of omeprazole. Interday and intraday precision did not exceed 10%, and the range of accuracy values were from −1.43% to 2.76%. The results of extraction recovery and stability met the requirements of FDA approval guidelines of bioanalytical method validation. The Cmax of omeprazole in group B was 61.55% higher than that in group A, and the AUC(0−t) and AUC(0−∞) of omeprazole in group B were 63.96% and 63.65% higher those that in group A, respectively. At the same time, the clearance (CL) and apparent volume of distribution (Vd) decreased in group B. In this study, an HPLC method for the determination of plasma omeprazole concentration was established. SJZPs could inhibit the metabolism of omeprazole and increase the concentration of omeprazole in beagle dogs. It is suggested that when SJZPs are combined with omeprazole, attention should be paid to the herb-drug interactions and possible adverse reactions.



2019 ◽  
Vol 1 (1) ◽  
pp. 104-109
Author(s):  
Suset J. Tolentino-Hernández ◽  
Leticia Cruz-Antonio ◽  
Irma Torres-Roque ◽  
Jose T. Pérez-Urizar

Background. There are numerous reports of low-quality formulations of ciprofloxacin in the market, which has been associated with therapeutic failure and the development of microbial resistance. Objective. The aim of this study is evaluating the bioequivalence between two oral immediate-release ciprofloxacin 250 mg tablets. Material and Methods. The study was performed in 24 Mexican healthy volunteers following a randomized cross over 2 × 2 design. Single doses of a test formulation Lemyflox® (Lemery Laboratories, Mexico) and the reference formulation Ciproxina® (Bayer, Mexico) were administered; blood samples were obtained during a 12 h period. Ciprofloxacin plasma concentrations were quantified using a validated High-Pressure Liquid Chromatography (HPLC) method, plasma concentration against time curves were constructed and pharmacokinetic parameters were determined by non-compartmental analysis. In order to determine bioequivalence, test/reference ratios of Cmax, AUC0-t and AUC0-inf were compared using analysis of variance (ANOVA), followed by the 90 % confidence intervals and the Schuirmann bilateral test. Results. The 90 % confidence intervals limits ranged from 82.92 to 100.88 % for Cmax, from 93.05 to 109.15 % for AUC0-t and from 97.76 to 114.99 % for AUC0-inf, all cases were within bioequivalence acceptance range of 80 - 125 %. Schuirmann test confirmed such observation as the probability that Cmax, AUC0-t and AUC0-inf ratios were beyond 80 - 125 % was lower than 0.05. Conclusions. The results obtained demonstrate bioequivalence between the test and reference formulations.



1993 ◽  
Vol 39 (2) ◽  
pp. 263-271 ◽  
Author(s):  
T Fiskerstrand ◽  
H Refsum ◽  
G Kvalheim ◽  
P M Ueland

Abstract We have developed a modified version of our fully automated column-switching HPLC method for determining total plasma homocysteine based on single-column (reversed-phase) separation. Homocysteine, cysteine, and cysteinylglycine in plasma (total concentrations), acid-precipitated plasma (non-protein-bound concentrations), and urine can be determined. The derivatization and chromatography were performed automatically by a sample processor. The successful separation of all thiol species (within 15 min) was accomplished by accurate adjustment of the pH of the mobile phase to 3.65 (plasma) or 3.50 (acid-precipitated plasma, urine). Maximal fluorescence yield of cysteine, cysteinylglycine, and, to a lesser degree, homocysteine was dependent on optimal concentrations of EDTA and dithioerythritol during reduction (with NaBH4) and derivatization (with monobromobimane). The method is sensitive (detection limit approximately 0.05 pmol) and has a high degree of precision (CV < 5%). The sample output is approximately 70 samples in 24 h. Serum and heparin plasma can also be analyzed. Hemolysis up to approximately 2.0 g/L of hemoglobin did not interfere with the analytical recovery of homocysteine or cysteine. Collection of blood, separation of plasma from whole blood, and acid precipitation must be standardized to obtain reproducible thiol results. Our modifications and the standardization of blood-sampling procedures have substantially improved the method and broadened its applications.



Author(s):  
Wael Abu Dayyih ◽  
Lina Tamimi ◽  
Eyad Mallah ◽  
Kenza Mansour ◽  
Tawfiq Arafat ◽  
...  

Objective: It is to develop a simple, valid and rapid chromatographic method for quantification of saxagliptin in rats serum in order to study saxagliptin pharmacokinetic parameters in sucralose fed rats simultaneously to detect any interaction possibility between saxagliptin and sucralose in rats. Methods: In our developed method of analysis, mobile phase consisted of phosphate buffer (pH =4) and methanol (70:30) v/v at flow rate of 1 ml/min with UV detection at 230 nm., C8 column of separation was used with temperature of 40 C ° using injection volume of 50 µl, samples run time was 10 min, and sildenafil citrate was used as internal standard. saxagliptin was given to rats orally of (2g/kg) dose while sucralose was given with (11 mg/kg/day) dose.Results: A successful HPLC method was validated and developed to determine saxagliptin in rats serum, overall intra-day precision and accuracy were reasonable with coefficient of variation percentage CV % values range (o.14-4.03) and accuracy % range (99.5-104), while inter-day precision and accuracy showed accepted precision with CV% range (0.15-2.81) and accuracy % range (99.9-116). The coefficient of correlation was 0.99949 with reasonable sensitivity and selectivity. Combination effect of saxagliptin with sucralose on saxagliptin serum profile was demonstrated as strong statistical effect according to Cohen’s d and significant P values too.Conclusion: A successful HPLC method was validated and developed to quantify saxagliptin in rats serum, combination effect of saxagliptin with sucralose over all time intervals of saxagliptin serum profile was demonstrated as strong statistical effect.



Author(s):  
Satish Puttachari ◽  
Navanath. V. Kalyane ◽  
Sarbani Duttagupta

Cefuroxime axetil has poor bioavailability due to low solubility. This can be surmounted by preparing the drug by self-microemulsifying drug delivery system (SMEDDS). In this study the bioavailability of cefuroxime axetil from SMEDDS and tablets was evaluated in Wistar rats. The optimized SMEDDS formulation was prepared using Labrasol®, Gelucire® 44/14 and Lutrol®E400. The formulation was evaluated for micro-emulsification properties and percent in-vitro dissolution. The HPLC method was developed and optimized to estimate the drug content in the plasma. The method was clearly separating the cefuroxime A and B polymorphs and LOD and LOQ values are satisfactory. Rats were randomized in to two groups - one group of animals were administered with SMEDDS and another with tablet formulation. At frequent intervals the blood samples were withdrawn and analysed for drug content. The pharmacokinetic parameters were calculated using PK Solve software. The calculated bioavailability and tmax from SMEDDS was 1687.06 μg/ mL.min and 50 min, respectively, whereas for tablet it was  1219.803 μg/mL.min and 62 minutes, respectively. The bioavailability of SMEDDS formulation was 1.5 times more than the marketed formulation, indicating a significant improvement in oral bioavailability. In conclusion, this study confirms that the SMEDDS formulation is a viable strategy for enhancing the oral bioavailability of cefuroxime axetil



Author(s):  
Khater Ahmed Saeed AL-Japairai ◽  
Bappaditya Chatterjee ◽  
Syed Mahmood ◽  
Samah Hamed Almurisi

The telmisartan was determined in a rat plasma using developed and validated a reversed-phase high performance liquid chromatographic (HPLC). The pre-treatment of the plasma sample involving liquid-liquid extraction using ethanol as the extracting solvent. The HPLC method validation has been shown a linear calibration curve over a plasma concentrations range of 0.7 to 10µg/mL with a correlation coefficient of 0.9979, the limit of detection and the limit of quantification were determined to be 0.025µg/ml and 0.07µg/ml, respectively. The precision and accuracy were in an acceptable limit. The pharmacokinetic parameters of telmisartan were adequately evaluated following a single oral dose (4mg/kg) in Sprague-Dawley rats. The results observed conclude that the developed bioanalytical HPLC method is appropriate and applicable as an analytical tool in the pharmacokinetic study of telmisartan.



2007 ◽  
Vol 1304 ◽  
pp. 415-419 ◽  
Author(s):  
K. Kawai ◽  
H. Ishikawa ◽  
K. Ohashi ◽  
Y. Itoh ◽  
R. Teradaira


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