STANDARDIZATION OF HYGROPHILA SPINOSA AND ITS FORMULATION WITH REFERENCE TO LUPEOL, BY DEVELOPED AND VALIDATED HPTLC AND RP-HPLC METHODS

INDIAN DRUGS ◽  
2015 ◽  
Vol 52 (01) ◽  
pp. 13-19
Author(s):  
R Jayaprakasam ◽  
◽  
M. F. Saleshier ◽  
T. K. Ravi
Keyword(s):  
Standard Deviation ◽  
Ethyl Acetate ◽  
Mobile Phase ◽  
Solvent System ◽  
Good Recovery ◽  
Rp Hplc ◽  
Relative Standard ◽  
Optimum Wavelength ◽  
Hptlc Method

The separation and determination of lupeol from Hygrophila spinosa were carried out by two simple, precise and accurate HPTLC and RP-HPLC methods. HPTLC method for the determination of lupeol from plant extract and its formulation was developed using a solvent system consisting of toluene : ethyl acetate : methanol (15: 3: 1.5%v/v/v). For detection, lupeol had to be derivatized with Liebermann Burchard reagent at 1050C. The optimum wavelength was fixed as 366nm. In RP-HPLC, the separation was carried out on a C18 column and the mobile phase selected was methanol: acetonitrile (30:70%v/v). The maximum wavelength was found to be 210nm.The method was validated in terms of various parameters. Low relative standard deviation and good % recovery values of both the methods showed that the developed methods were highly precise and accurate and therefore can be used for the standardization and quantification of lupeol in Hygrophila spinosa and its formulation.

scholarly journals Development and validation of reversed phase high performance liquid chromatography (RP-HPLC) for quantification of captopril in rabbit plasma

2020 ◽  
Author(s):  
Muhammad Fawad Rasool ◽  
Umbreen Fatima Qureshi ◽  
Nazar Muhammad Ranjha ◽  
Imran Imran ◽  
Mouqadus Un Nisa ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Mobile Phase ◽  
High Performance ◽  
Limit Of Detection ◽  
Reversed Phase ◽  
Rabbit Plasma ◽  
Rp Hplc ◽  
Relative Standard

AbstractTh accurate rapid, simple and selective reversed phase high performance liquid chromatography (RP-HPLC) has been established and validated for the determination of captopril (CAP). Chromatographic separation was accomplished using prepacked ODSI C18 column (250 mm × 4.6 mm with 5 μm particle size) in isocratic mode, with mobile phase consisting of water: acetonitrile (60:40 v/v), pH adjusted to 2.5 by using 85% orthophosphoric acid at a flow rate of 1 mL/min and UV detection was performed at 203 nm. RP-HPLC method used for the analysis of CAP in mobile phase and rabbit plasma was established and validated as per ICH-guidelines. It was carried out on a well-defined chromatographic peak of CAP was established with a retention time of 4.9 min and tailing factor of 1.871. The liquid–liquid extraction method was used for extraction of CAP from the plasma. Excellent linearity (R2 = 0.999) was shown over range 3.125–100 µg/mL with mean percentage recoveries ranges from 97 to 100.6%. Parameters of precision and accuracy of the developed method meet the established criteria. Intra and inter-day precision (% relative standard deviation) study was also performed which was less than 2% which indicate good reproducibility of the method. The limit of detection (LOD) and quantification for the CAP in plasma were 3.10 and 9.13 ng/mL respectively. The method was suitably validated and successfully applied to the determination of CAP in rabbit plasma samples.

RP-HPLC AND HPTLC STABILITY INDICATING ASSAY METHODS FOR IVERMECTIN IN BULK AND TABLET DOSAGE FORM

INDIAN DRUGS ◽  
2018 ◽  
Vol 55 (03) ◽  
pp. 32-42
Author(s):  
G. P Wani ◽  
◽  
S. B Jadhav
Keyword(s):  
Mobile Phase ◽  
Stress Testing ◽  
Hplc Method ◽  
Rp Hplc ◽  
Assay Methods ◽  
Photo Stability ◽  
Tablet Dosage ◽  
Hptlc Method ◽  
Alkaline Oxidation

Simple, rapid, precise, accurate RP-HPLC and HPTLC methods have been developed and validated for ivermectin in bulk and its marketed formulation. RP-HPLC method for drug was achieved on Grace C18 (250 mm X 4.6 ID, Particle size; 5 μ) column using mobile phase acetonitrile: 10 mM phosphate buffer (95:05 v/v) pH adjusted to 3 with o-phosphoric acid. Detection of drug was done at 245 nm. The retention time was found to be 5.83 min. HPTLC method for ivermectin was accomplished on a precoated silica gel aluminium plate 60F-254 (CAMAG Linomat 5), using toluene: methanol: glacial acetic acid (8:2:0.1 v/v/v) as a mobile phase. The densitometric scanning was performed at 245 nm which showed Rf 0.46 for ivermectin. The stress testing of the drug individually was carried out under acidic, alkaline, oxidation, photo-stability and thermal degradation conditions. The proposed methods were successfully applied for the determination of drug in bulk and its marketed formulation.

scholarly journals Determination of Patulin in Apple Juice by Liquid Chromatography

2006 ◽  
Vol 89 (1) ◽  
pp. 139-143 ◽  
Author(s):  
Maria Helena Iha ◽  
Myrna Sabino
Keyword(s):  
Liquid Chromatography ◽  
Standard Deviation ◽  
Mobile Phase ◽  
Apple Juice ◽  
Array Detector ◽  
Diode Array ◽  
Diode Array Detector ◽  
Relative Standard ◽  
Precision Study

Abstract A method was developed and validated in-house for the determination of patulin (PAT), a toxic mold metabolite, in apple juice. The sample was extracted with ethyl acetatehexane and analyzed by liquid chromatography equipped with a C18 column and diode array detector. The mobile phase used for the quantification was waterethanol, at a flow rate of 0.5 mL/min. The method showed a mean recovery of 84.8%, the relative standard deviation obtained in the precision study was <7.7%, the quantification and detection limits were 7 and 3 μg/L, respectively, and the linear range for PAT in apple juice was 2.6650 μg/L. The ruggedness was evaluated by an intralaboratory experiment, in which 5 factors were studied, and only one was found to influence the observed results. The developed method is fast, practical, and simple; the solvents (except hexane) and reagents used were nontoxic. The results of the validation confirmed the efficiency of the method, which is sensitive enough to be used in studies required to quantify PAT in apple juice.

scholarly journals Determination of Delafloxacin in Pharmaceutical Formulations Using a Green RP-HPTLC and NP-HPTLC Methods: A Comparative Study

Antibiotics ◽  
2020 ◽  
Vol 9 (6) ◽  
pp. 359 ◽  
Author(s):  
Prawez Alam ◽  
Essam Ezzeldin ◽  
Muzaffar Iqbal ◽  
Gamal A.E. Mostafa ◽  
Md. Khalid Anwer ◽  
...  
Keyword(s):  
Ethyl Acetate ◽  
Silica Gel ◽  
Solid Lipid Nanoparticles ◽  
Ternary Mixture ◽  
Mobile Phase ◽  
Pharmaceutical Formulations ◽  
Lipid Nanoparticles ◽  
Ammonia Solution ◽  
Hptlc Method

In this work; delafloxacin (DLFX) was determined using a validated green RP-HPTLC and NP-HPTLC methods in commercial tablets and in-house developed solid lipid nanoparticles (SLNs). RP-HPTLC determination of DLFX was performed using “RP-18 silica gel 60 F254S HPTLC plates”. However; NP-HPTLC estimation of DLFX was performed using “silica gel 60 F254S HPTLC plates”. For a green RP-HPTLC method; the ternary combination of ethanol:water:ammonia solution (5:4:2 v/v/v) was used as green mobile phase. However; for NP-HPTLC method; the ternary mixture of ethyl acetate: methanol: ammonia solution (5:4:2 v/v/v) was used as normal mobile phase. The analysis of DLFX was conducted in absorbance/reflectance mode of densitometry at λmax = 295 nm for both methods. RP-HPTLC method was found more accurate, precise, robust and sensitive for the analysis of DLFX compared with the NP-HPTLC method. The % assay of DLFX in commercial tablets and in-house developed SLNs was determined as 98.2 and 101.0%, respectively, using the green RP-HPTLC technique, however; the % assay of DLFX in commercial tablets and in-house developed SLNs was found to be 94.4 and 95.0%, respectively, using the NP-HPTLC method. Overall, the green RP-HPTLC method was found superior over the NP-HPTLC. Therefore, the proposed green RP-HPTLC method can be successfully applied for analysis of DLFX in commercial tablets, SLNs and other formulations containing DLFX.

Medium-pressure liquid chromatography of platinum metal ions on Spheron DEAE

1983 ◽  
Vol 48 (8) ◽  
pp. 2255-2262 ◽  
Author(s):  
František Vláčil ◽  
Ivan Vinš ◽  
Oldřich Malíček
Keyword(s):  
Liquid Chromatography ◽  
Standard Deviation ◽  
Metal Ions ◽  
Mobile Phase ◽  
Platinum Metal ◽  
Hydrochloric Acid Concentration ◽  
Chloride Medium ◽  
Relative Standard ◽  
Medium Pressure Liquid Chromatography

Spheron DEAE (modified macroreticular hydroxyethylmethacrylate-ethylenedimethacrylate copolymer) was used for chromatographic separation and determination of Rh(III), Pd(II), and Pt(IV) in chloride medium. The most suitable composition of the mobile phase was looked for by studying the influence of hydrochloric acid concentration on the capacity ratios of the metal ions mentioned and on their resolution, as well as the influence of different additions to the mobile phase on the decrease of the high Pt(IV) retention. Using the photometric (UV) detection, the linear dependence was found up to following concentrations: Rh 200 mg l-1, Pd 2 g l-1, Pt 500 mg l-1. The detection limit was 23 ng Rh, 62 ng Pd and 96 ng Pt in 7 μl sample injected.The reproducibility of the determination was (as relative standard deviation for n = 3) 1-4%, relative error 0.7-7%.

scholarly journals SIMULTANEOUS DETERMINATION OF PARACETAMOL AND IBUPROFENE MIXTURES BY HIGH PERFORMANCE LIQUID CHROMATOGRAPHY

2010 ◽  
Vol 3 (1) ◽  
pp. 9-13 ◽  
Author(s):  
Sophi Damayanti ◽  
Slamet Ibrahim ◽  
Kurnia Firman ◽  
Daryono H Tjahjono
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Standard Deviation ◽  
Retention Time ◽  
Analytical Method ◽  
Phosphate Buffer ◽  
Mobile Phase ◽  
High Performance ◽  
Relative Standard

Analytical method for the determination of paracetamol and ibuprofene mixtures has been developed by High Performance Liquid Chromatography using C-18 column and acetinitrile - phosphate buffer pH = 4.5 (75:25) containing 0.075% sodium hexanesulfunate as a mobile phase. The detector was set at 215 nm. Using such conditions, retention time for paracetamol and ibuprofen was 4.89 and 7.11 min, respectively. The recovery for paracetamol and ibuprofen was found to be 101.07± 0.73% and 102.02 ± 1.58%, respectively. The detector limits of the method was 1.30 and 1.60 μg/mL with the relative standard deviation (RSD) 0.74 and 1.52% for paracetamol and ibuprofen, respectively.   Keywords: paracetamol, ibuprofen, multi-component, validation, HPLC.

Rapid Determination of Deoxynivalenol (Vomitoxin) by Liquid Chromatography Using Modified Romer Column Cleanup

1984 ◽  
Vol 67 (1) ◽  
pp. 52-54 ◽  
Author(s):  
Henry L Chang ◽  
Jonathan W Devries ◽  
Paul A Larson ◽  
Hasmukh H Patel
Keyword(s):  
Liquid Chromatography ◽  
Standard Deviation ◽  
Mobile Phase ◽  
Rapid Determination ◽  
Alumina Column ◽  
Relative Standard ◽  
Alumina Column Chromatography ◽  
Wheat Products ◽  
Liquid Chromatographic

Abstract A modification of the Romer method for determining deoxynivalenol (DON) provides rapid sample cleanup and includes liquid chromatographic (LC) quantitation. The method was evaluated using wheat, wheat flour, and other wheat products. The sample is extracted with acetonitrile–water (84 + 16), and an aliquot of the extract is subjected to activated charcoal–alumina column chromatography. The extract is then evaporated and diluted to volume with mobile phase, and DON is quantitated using liquid chromatography. The relative standard deviation based on duplicate samples is 6.07%. The detection limit is 30 ppb based on 2 x signal/noise ratio. Results by this method compared with the results obtained by the Scott GC method showed a correlation coefficient of 0.992 with a mean vomitoxin content of 779 ppb by this method and 716 ppb by the Scott method for 14 samples.

scholarly journals Stability-indicating RP-HPLC method for determination of beclomethasone dipropionate in nanocapsule suspensions

2015 ◽  
Vol 51 (4) ◽  
pp. 803-810 ◽  
Author(s):  
Janaíne Micheli Chassot ◽  
Luana Mota Ferreira ◽  
Felipe Pereira Gomes ◽  
Letícia Cruz ◽  
Leandro Tasso
Keyword(s):  
Mobile Phase ◽  
Beclomethasone Dipropionate ◽  
Degradation Products ◽  
Degradation Kinetics ◽  
Hplc Method ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Relative Standard ◽  
Bulk Drug

abstract A simple stability-indicating RP-HPLC/UV method was validated for determination of beclomethasone dipropionate (BD) in nanocapsule suspensions. Chromatographic conditions consisted of a RP C18column (250 mm x 4.60 mm, 5 µm, 110 Å), using methanol and water (85:15 v/v) as mobile phase at 1.0 mL/min with UV detection at 254 nm. The calibration curve was found to be linear in the concentration range of 5.0-25.0 µg/mL with a correlation coefficient > 0.999. Precision was demonstrated by a relative standard deviation lower than 2.0%. Accuracy was assessed by the recovery test of BD from nanocapsules (98.03% to 100.35%). Specificity showed no interference from the components of nanocapsules or from the degradation products derived from acid, basic and photolytic conditions. In conclusion, the method is suitable to be applied to assay BD in bulk drug and in nanocapsules, and it can be employed to study stability and degradation kinetics.

scholarly journals Simultaneous Determination of Rutin, Luteolin, Quercetin, and Betulinic Acid in the Extract ofDisporopsis pernyi(Hua) Diels by UPLC

2015 ◽  
Vol 2015 ◽  
pp. 1-5 ◽  
Author(s):  
Yanqi Wang ◽  
Shuyi Li ◽  
Dandan Han ◽  
Kehan Meng ◽  
Miao Wang ◽  
...  
Keyword(s):  
Quality Control ◽  
Liquid Chromatography ◽  
Standard Deviation ◽  
Betulinic Acid ◽  
Mobile Phase ◽  
Gradient Elution ◽  
Ultra Performance Liquid Chromatography ◽  
Relative Standard ◽  
Quantitative Basis

Disporopsis pernyi(Hua) Diels, which belongs to genusDisporopsis, has been widely used for the treatment of abnormal sweating, chronic cough, and so forth. An ultra-performance liquid chromatography (UPLC) analysis was developed for the determination of rutin, luteolin, quercetin, and betulinic acid inDisporopsis pernyi(Hua) Diels roots. UPLC analysis was conducted by using a Shim-pack XR-ODS column with gradient elution with the mobile phase of acetonitrile and water containing 0.1% formic acid and with a flow rate of 0.2 mL/min, detected at 210, 254, and 280 nm. The method was precise, with relative standard deviation < 2.0%. The recoveries for the four components inDisporopsis pernyi(Hua) Diels were between 98.5 and 100.9%. The average contents of rutin, luteolin, quercetin, and betulinic acid in roots were 5.63, 2.51, 3.87, and 2.41 μg/g, respectively. The method was accurate and reproducible and it can provide a quantitative basis for quality control ofDisporopsis pernyi(Hua) Diels.

Rapid determination of fosetyl-aluminium in commercial pesticide formulations by high-performance liquid chromatography

2014 ◽  
Vol 68 (6) ◽  
Author(s):  
Helen Karasali ◽  
Konstantinos Kasiotis ◽  
Kyriaki Machera
Keyword(s):  
Standard Deviation ◽  
Relative Standard Deviation ◽  
High Performance ◽  
Limit Of Detection ◽  
Rapid Determination ◽  
Hplc Method ◽  
Negative Ion ◽  
Rp Hplc ◽  
Relative Standard

AbstractAn isocratic reversed-phase high-performance liquid chromatographic (RP-HPLC) method with diode array detection (DAD) was developed for the determination of aluminium tris(ethyl phosphonate) (fosetyl-aluminium, fosetyl-Al) in plant-protection products. The method involves extraction of the active ingredient by sonication of the sample with water and direct measurement by RPHPLC. The isocratic RP-HPLC method for the analysis of fosetyl-Al thus developed was then validated for specificity, linearity, precision, and accuracy. The chromatographic peak confirmation was performed by LC-MS using electron spray ionisation in the negative-ion mode. The repeatability of the method, expressed as relative standard deviation (RSD, %), was found to be 0.5 % and the limit of detection was 0.035 mg mL−1. The average recoveries of the three fortification levels varied from 96.7 % to 100.6 % and the RSDs ranged between 2.6 % and 6.3 %. The precision of the method was also considered to be acceptable as the experimental repeatability relative standard deviation (RSDr) was lower than the RSDr, calculated using the Horwitz equation. The method is rapid, simple, accurate, cost-effective, and provides a new and reliable means for the analysis of fosetyl-Al in formulated products.

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