DETERMINATION THE CONCENTRATION OF ASIATICOSIDE IN CENTELLA ASIATICA (L.) URB. – APIACEAE AT QUANG DIEN DISTRICT, THUA THIEN HUE PROVINCE

2015 ◽  
pp. 63-68
Author(s):  
Thi Cam Minh Dao ◽  
Viet Khan Nguyen ◽  
Huu Tien Nguyen ◽  
Thi Thanh Ngoc Le ◽  
Viet Duc Ho

Background: Centella asiatica (L.) Urb. - Apiaceae has been used in traditional medicine to cure many diseases such as cholera dysentery, pimples, discharge, cough, sore throat, hemorrhoids and detoxification. The objective is to determine the amount of active ingredient asiaticoside in Centella asiatica (L.) Urb at Quang Tho 2 cooperatives, Quang Dien District, Thua Thien Hue province. Materials and method: C.asiatica after being harvested, washed and drained was dried in sunlight or in dryer with different temperature. Each 20g of C.asiatica was extracted using various methods with dissolving appropriate solvents. The extracted solution was diluted by extracted solvent. This diluted solution was filtered through 0.45μm membrane filter for the purpose of chromatography. Results: The chromatography condition: mobile phase consisting of methanol: Trifluoracetic acid 1% (60: 40); Column: HiQ Sil C18 (4.6 x 250 mmm) 3μm; flow rate at 0.7 ml/min; The maximum detection wavelength: 215 nm; retention time of asiaticosid (tR): 18.7 minutes. Conclusion: The content of asiaticoside in sample is from 0.09% to 1.35% depending on the initial sample handling and sample extraction method. Keywords: Centella asiatica (L.) Urb. - Apiaceae, asiaticoside, HPLC.

2019 ◽  
Vol 15 (6) ◽  
pp. 574-579
Author(s):  
Muhammad Ubaid ◽  
Mahmood Ahmad ◽  
Farhan Ahmad Khan ◽  
Ghulam Murtaza

Objective:This study was aimed at conducting a pharmacokinetic evaluation of metformin in rabbit plasma samples using rapid and sensitive HPLC method and UV detection.Methods:Acetonitrile was used for protein precipitation in the preparation of plasma samples. Reverse phase chromatography technique with silica gel column (250 mm × 4.6 mm, 5 μm) at 30°was used for the separation purpose. Methanol and phosphate buffer (pH 3.2) mixture was used as a mobile phase with flow rate 0.8 ml/min. The wavelength of UV detector was adjusted at 240 nm.Results:The calibration curve was linear in a range of 0.1-1 µg/ml with R² = 0.9982. The precision (RSD, %) values were less than 2%, whereas, accuracy of method was higher than 92.37 %. The percentage recovery values ranged between 90.14 % and 94.97 %. LOD and LOQ values were 25 ng/ml and 60 ng/ml, respectively. Cmax and AUC0-t values were found to be 1154.67 ± 243.37 ng/ml and 7281.83 ± 210.84 ng/ml.h, respectively after treating rabbits with a formulation containing 250 mg metformin.Conclusion:Based on the above findings, it can be concluded that present method is simple, precise, rapid, accurate and specific and thus, can be efficiently used for the pharmacokinetic study of metformin.


2018 ◽  
Vol 15 (1) ◽  
pp. 32-38 ◽  
Author(s):  
Bürge Aşçı ◽  
Mesut Koç

Introduction:This paper presents the development and validation of a novel, fast, sensitive and accurate high performance liquid chromatography (HPLC) method for the simultaneous quantitative determination of dibucaine HCl, fluocortolone pivalate and fluocortolone caproate in pharmaceutical preparations.Experiment:Development of the chromatographic method was based on an experimental design approach. A five-level-three-factor central composite design requiring 20 experiments in this optimization study was performed in order to evaluate the effects of three independent variances including mobile phase ratio, flow rate and amount of acid in the mobile phase.Conclusion:The optimum composition for mobile phase was found as a methanol:water:acetic acid mixture at 71.6 : 26.4 : 2 (v/v/v) ratio and optimum separation was acquired by isocratic elution with a flow rate of 1.3 mL/min. The analytes were detected using a UV detector at 240 nm. The developed method was validated in terms of linearity, precision, accuracy, limit of detection/quantitation and solution stability and successfully applied to the determination of dibucaine HCl, fluocortolone pivalate and fluocortolone caproate in pharmaceutical topical formulations such as suppositories and ointments.


Separations ◽  
2021 ◽  
Vol 8 (1) ◽  
pp. 5
Author(s):  
Mohd Afzal ◽  
Mohd. Muddassir ◽  
Abdullah Alarifi ◽  
Mohammed Tahir Ansari

A highly specific, accurate, and simple RP-HPLC technique was developed for the real-time quantification of domperidone (DOMP) and lansoprazole (LANS) in commercial formulations. Chromatographic studies were performed using a Luna C8(2), 5 μm, 100Å, column (250 × 4.6 mm, Phenomenex) with a mobile phase composed of acetonitrile/2 mM ammonium acetate (51:49 v/v), pH 6.7. The flow rate was 1 mL·min−1 with UV detection at 289 nm. Linearity was observed within the range of 4–36 µg·mL−1 for domperidone and 2–18 µg·mL−1 for lansoprazole. Method optimization was achieved using Box-Behnken design software, in which three key variables were examined, namely, the flow rate (A), the composition of the mobile phase (B), and the pH (C). The retention time (Y1 and Y3) and the peak area (Y2 and Y4) were taken as the response parameters. We observed that slight alterations in the mobile phase and the flow rate influenced the outcome, whereas the pH exerted no effect. Method validation featured various ICH parameters including linearity, limit of detection (LOD), accuracy, precision, ruggedness, robustness, stability, and system suitability. This method is potentially useful for the analysis of commercial formulations and laboratory preparations.


1977 ◽  
Vol 23 (12) ◽  
pp. 2288-2291 ◽  
Author(s):  
P H Culbreth ◽  
I W Duncan ◽  
C A Burtis

Abstract We used paired-ion high-performance liquid chromatography to determine the 4-nitrophenol content of 4-nitrophenyl phosphate, a substrate for alkaline phosphatase analysis. This was done on a reversed-phase column with a mobile phase of methanol/water, 45/55 by vol, containing 3 ml of tetrabutylammonium phosphate reagent per 200 ml of solvent. At a flow rate of 1 ml/min, 4-nitrophenol was eluted at 9 min and monitored at 404 nm; 4-nitrophenyl phosphate was eluted at 5 min and could be monitored at 311 nm. Samples of 4-nitrophenyl phosphate obtained from several sources contained 0.3 to 7.8 mole of 4-nitrophenol per mole of 4-nitrophenyl phosphate.


2006 ◽  
Vol 3 (1) ◽  
pp. 60-64 ◽  
Author(s):  
P. Venkata Reddy ◽  
B. Sudha Rani ◽  
G. Srinu Babu ◽  
J. V. L. N. Seshagiri Rao

A reverse phase HPLC method is developed for the determination of Raloxifene in pharmaceutical dosage forms. Chromatography was carried out on an inertsil C18 column using a mixture of acetonitrile and phosphate buffer (30:70 v/v) as the mobile phase at a flow rate of 1 mL/min. Detection was carried out at 290 nm .The retention time of the drug was 10.609 min. The method produced linear responses in the concentration range of 0.5-200 µg/mL of Raloxifene. The method was found to be applicable for determination of the drug in tablets.


INDIAN DRUGS ◽  
2019 ◽  
Vol 56 (07) ◽  
pp. 59-68
Author(s):  
H Mahajan ◽  
S Savale ◽  
P Nerkar ◽  

The present study was aimed at developing a Reversed-Phase High-Performance Liquid Chromatography (RP-HPLC) method for simultaneous determination of curcumin (CRM) and gefitinib (GFT) in bulk, plasma and brain homogenate. hydrochlorothiazide was used as an internal standard (IS). A new simple, rapid, selective, precise and accurate RP-HPLC method has been developed. The separation was achieved by using C-18 column (Qualisil BDS C18, 250 mm x 4.6 mm I.D.) coupled with a guard column of silica, mobile phase consisted of acetonitrile: water with 0.1% formic acid (30:70 v/v). The flow rate was 0.2 ml/min and the drug was detected using PDA detector at the wavelength of 242 nm. The experimental conditions, including the diluting solvent, mobile phase composition, column saturation and flow rate, were optimised to provide high-resolution and reproducible peaks. The method was developed and tested for linearity range of 10-60 μg/mL for bulk analysis and 200-800 ng/mL for plasma and brain homogenate. The developed method was validated as per ICH guidelines, in terms of linearity, application of the proposed method to bulk sample, recovery, precision, repeatability, ruggedness, sensitivity (LOD and LOQ) and robustness and stability study (short and long-term stabilities, freeze/thaw stability, post-preparative). The low value of % RSD showed that the method was precise within the acceptance limit of 2%. The developed method was successfully applied for the analysis of the drug in bulk as well as various marketed formulation and drug in plasma and brain distribution studies.


2020 ◽  
pp. 1-14
Author(s):  
Dina El Sherbiny ◽  
Mary E. K. Wahba

Abstract A simple HPLC technique has been utilized for rapid and sensitive quantitative analysis of two mixtures of drugs that are used during pregnancy and lactation. Drugs of the first mixture are used to manage gastrointestinal tract illness that are common during early stages of pregnancy, while pharmaceutical agents of the second mixture are administered over the counter as galactagogues or to overcome postpartum depression. Mixture I includes famotidine (FMT), ranitidine (RNT), nizatidine (NZT), and pantoprazole (PNT), which were separated on a C18 column using a mobile phase composed of methanol: 0.02 M sodium dihydrogen phosphate (60:40, v/v) of pH 6.9, adopting UV detection at 240 nm at a flow rate of 1 mL/min. Mixture II on the other hand, consists of domperidone (DOM), metoclopramide (MET), and sulpiride (SUL). These drugs were eluted using the same column and flow rate as those in mixture I, using a mobile phase consisting of acetonitrile: 0.075 M sodium dihydrogen phosphate (30:70, v/v) of pH 6 adopting a detection wavelength 270 nm. Two optimization protocols were utilized to optimize the chromatographic separation conditions, namely one factor at a time (OFAT) and design of experiments (DOE) where face centered cube response surface experimental design was chosen for this investigation. Comparison of the results obtained from both protocols reveals the accordance between them. Full validation procedure under guidance of United States Pharmacopoeia (USP) was applied to the proposed methods which enabled their application to separate the drugs of both mixtures in spiked rat whole blood samples and in vivo analysis of rat heart blood.


2013 ◽  
Vol 821-822 ◽  
pp. 1005-1008
Author(s):  
Li Min Ma ◽  
Li Cui ◽  
Yu Hang Zhao

Detection of 9а-OH-AD prepared by biotransformation by RP-HPLC directly was studied.The detection is performed on a Kromasil 100-5C18(4.6×250mm) column, using methanol:water(7:3,v/v)as mobile phase,0.8mL•min-1flow rate and external standard method,deteced at 242nm.There is a good line correlaction between peak and content in range of 0.01-0.20g/L,the correlation coefficient is 0.9942,the average recovery is 99.09% with a relative stand deviation of 0.89%(n=5).The method is simple,stable,accurate and reliable for quality control of 9а-OH-AD.


2021 ◽  
Vol 33 (11) ◽  
pp. 2723-2728
Author(s):  
Surya Prakash Mamillapalli ◽  
Gourabattina Lakshmi Prasanna ◽  
B. Venkata Subbaiah ◽  
N. Annapurna

Stability indicating reversed phase-HPLC method for simultaneous estimation of mometasone furoate (MAF) and formoterol fumarate (FFD) in metered dose inhalation aerosol (MDI) dosage formulation has been developed and discussed in the present work. The chromatographic separation was achieved using Hypersil ODS column (250 mm × 4.6 mm, 3 μm) using an isocratic separation mode at a flow rate of 1.2 mL/min, column temperature of 50 ºC. The system operates with a mobile phase comprising of solution-A (buffer): Solution-B (acetonitrile) mixed in the ratio of 70:30 %v/v at a UV detection wavelength of 214 nm. Retention times of mometasone furoate and formoterol fumarate found to be about 3 min and 7 min, respectively. All possible degradation products of both compounds were monitored at 214 nm and spectral purity along with % mass balance is assessed using PDA detector. Both analyte were subjected to force degradation studies, found all degradants were resolved from analyte peaks and also other process-related impurities. The proposed method is validated for specificity, linearity, accuracy, precision and robustness as per ICH guidelines and found to be adequate. Method stood to be robust with variation in column temperature, flow rate, pH of buffer and organic content in mobile phase.


Author(s):  
Sridatla V.V.S.S.N. Raju ◽  
S. Venkat Rao ◽  
A. Manikandan

A delicate, fast, Accurate, exact and steadiness, showing isocratic RP-UPLC method was developed for the concurrent assurance of the Ceftazidime and Avibactam in bulk and formulation. To optimize, a column HSS C18 100 x 2.1mm, 1.8µm, Mobile phase containing water: acetonitrile choose in the ratio 75:25v/v was pumped through column at a flow rate of 0.3ml/min at 260nm, initiate to be an efficient method for elution of drug with good peak shapes as well as retention times. Rt of Avibactam and Ceftazidime were initiate to be 1.463 min and 2.109 min. %Recovery was obtained as 100.07% and 100.08% for Avibactam and Ceftazidime separately. LOD, LOQ values got from relapse conditions of Avibactam and Ceftazidime were 0.85, 2.56 and 3.53, 10.70 correspondingly. Regression equation of Ceftazidime is y = 7883.2x + 12277, and y = 3279.1x + 1137 of Avibactam.


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