scholarly journals UHPLC-PDA Assay for Simultaneous Determination of Vitamin D3and Menaquinone-7 in Pharmaceutical Solid Dosage Formulation

2017 ◽  
Vol 2017 ◽  
pp. 1-9 ◽  
Author(s):  
Muhammad Jehangir ◽  
Mahmood Ahmed ◽  
Muhammad Imtiaz Shafiq ◽  
Abdul Samad ◽  
Iftikhar-ul-Haq
Keyword(s):  
Vitamin D ◽  
Simultaneous Determination ◽  
Hplc Method ◽  
Coefficient Of Determination ◽  
Solid Dosage ◽  
Mobile Phases ◽  
Relative Standard ◽  
Repeatability And Reproducibility ◽  
Ultrahigh Performance Liquid Chromatography

A newly developed method based on ultrahigh performance liquid chromatography (UHPLC) was optimized for the simultaneous determination of vitamin D3and menaquinone-7 (MK-7) in tablet formulation in the present study. UHPLC separation of vitamin D3and MK-7 was performed with ACE Excel 2 C18-PFP column (2 μm, 2.1×100 mm) at 0.6 mL min−1flow rate, whereas the mobile phase consisted of methanol/water (19:1, v/v, phase A) and isopropyl alcohol (99.9%, phase B) containing 0.5% triethylamine. Isocratic separation of both the analytes was performed at 40°C by pumping the mobile phases A and B in the ratio of50:50(v/v, pH, 6.0). Both analytes were detected at a wavelength of 265 nm and the injection volume was 1.0 μL. The overall runtime per sample was 4.5 min with retention time of 1.26 and 3.64 min for vitamin D3and MK-7, respectively. The calibration curve was linear from 5.0 to 100 μg mL−1for vitamin D3and MK-7 with a coefficient of determination (R2)≥0.9981, while repeatability and reproducibility (expressed as relative standard deviation) were lower than 1.46 and 2.21%, respectively. The proposed HPLC method was demonstrated to be simple and rapid for the determination of vitamin D3and MK-7 in tablets.

scholarly journals Stability-indicating RP-HPLC method for simultaneous determination of metformin hydrochloride and vildagliptin in tablet and biological samples

2020 ◽  
Vol 32 (1) ◽  
pp. 39-43
Author(s):  
Abdul Shakoor ◽  
Mahmood Ahmed ◽  
Rabia Ikram ◽  
Sajad Hussain ◽  
Arifa Tahir ◽  
...  
Keyword(s):  
Simultaneous Determination ◽  
Biological Samples ◽  
Degradation Products ◽  
Reversed Phase ◽  
Hplc Method ◽  
Coefficient Of Determination ◽  
Metformin Hydrochloride ◽  
Rp Hplc ◽  
Relative Standard

The present work aimed to develop and validate a simple, rapid, sensitive, accurate, and precise method for simultaneous determination of metformin hydrochloride and vildagliptin in tablet and biological samples. Isocratic elution of both the analytes was performed at 35 °C by injecting 20 μL into Thermo Hypersil ODS C18 column (5 μm, 4.6 mm× 250 mm), while the flow rate was set to 0.8 mL/min. The mobile phase comprised of methanol, acetonitrile, and phosphate buffer (5:30:65, v/v, pH 3.5), and wavelength was selected at 212 nm. The overall run time per sample was 7.0 min with a retention time of 3.36 and 5.41 min for metformin hydrochloride and vildagliptin, respectively. The calibration curve was linear from 10–140 μg/mL for metformin and 1–14 μg/mL for vildagliptin with a coefficient of determination (R2) ≤ 0.9919, while repeatability and reproducibility (expressed as relative standard deviation) were lower than 1.13 and 0.97%, respectively. Force degradation studies indicated a complete separation of the analytes in the presence of their degradation products providing a high degree of method specificity. The proposed reversed-phase high-performance liquid chromatography (RP-HPLC) method was demonstrated to be simple and rapid for the determination of metformin hydrochloride and vildagliptin in commercially available tablet and biological samples providing recoveries ranged between 100.13–100.29%.

scholarly journals Simultaneous determination of clobutinol hydrochloride and doxylamine succinate from syrups by RP HPLC using a new stationary phase containing embedded urea polar groups

2012 ◽  
Vol 48 (2) ◽  
pp. 315-323 ◽  
Author(s):  
Paulo Cesar Pires Rosa ◽  
Isabel Cristina Sales Fontes Jardim
Keyword(s):  
Stationary Phase ◽  
Simultaneous Determination ◽  
Reversed Phase ◽  
Hplc Method ◽  
Array Detector ◽  
Polar Groups ◽  
Ich Guidelines ◽  
Relative Standard ◽  
New Stationary Phase

A new, simple, fast, reproducible and sensitive reversed phase HPLC method, using a new stationary phase containing embedded urea polar groups, has been developed and validated for the simultaneous determination of clobutinol hydrochloride (CLO) and doxylamine succinate (DOX) in syrups. The determination was carried out on a C8 urea column (125 mm x 3.9 mm i.d., 5 µm particle size) synthetized at the Liquid Chomatography Laboratory (LabCrom) of the Chemistry Institute of Unicamp. The mobile phase consisted of a mixture of acetonitrile:methanol:phosphate buffer (pH 2.5) in the gradient mode. The diode array detector (DAD) was operated at 230 nm for CLO and 262 nm for DOX. The method showed adequate precision, with relative standard deviations (RSD) less than 1%. The presence of the excipients did not interfere in the results of the analysis. Accuracy was determined by adding standards of the drugs to a placebo and good recovery values were obtained. The analytical curves were linear (r² 0.9999 for CLO and 0.9998 for DOX) over a wide concentration range (2.4-336 µg mL-1 for CLO and 2.3-63 µg mL-1 for DOX). The solutions were stable for at least 72 hours at room temperature. The criteria for validation using the ICH guidelines were fulfilled.

scholarly journals Development and Validation of RP-HPLC Method for the Simultaneous Determination of Rabeprazole Sodium and Itopride Hydrochloride in Solid Dosage Form

2010 ◽  
Vol 7 (3) ◽  
pp. 947-952 ◽  
Author(s):  
Rajesh Sharma ◽  
Ganesh Prasad Mishra ◽  
Subhash Chandra Chaturvedi
Keyword(s):  
Simultaneous Determination ◽  
High Performance ◽  
Dosage Form ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Solid Dosage Form ◽  
Solid Dosage ◽  
Rabeprazole Sodium ◽  
Itopride Hydrochloride

A simple, sensitive, precise, accurate, rapid and reproducible reverse phase high performance liquid chromatographic procedure is developed for simultaneous determination of rabeprazole sodium and itopride hydrochloride in solid dosage form. The mobile phase used was a combination of acetonitrile: buffer (35:65 v/v) and the pH was adjusted to 7.0 ± 0.1 by addition of triethylamine. The detection of the capsule dosage form was carried out at 266 nm and a flow rate employed was 1 mL/min. Linearity was obtained in the concentration range of 2 to 16 μg/mL of rabeprazole sodium and 5 to 55 μg/mL of itopride hydrochloride with a correlation coefficient of 0.9992 and 0.9996 respectively. The results of the analysis were validated statistically and recovery studies confirmed the accuracy of the proposed method.

scholarly journals Stability-indicating HPLC-PDA assay for simultaneous determination of paracetamol, thiamine and pyridoxal phosphate in tablet formulations

2019 ◽  
Vol 69 (2) ◽  
pp. 249-259 ◽  
Author(s):  
Amir Ali ◽  
Muhammad Makshoof Athar ◽  
Mahmood Ahmed ◽  
Kashif Nadeem ◽  
Ghulam Murtaza ◽  
...  
Keyword(s):  
Simultaneous Determination ◽  
Pyridoxal Phosphate ◽  
Degradation Products ◽  
Ammonium Phosphate ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Complete Separation ◽  
Coefficient Of Determination ◽  
Tablet Formulations

Abstract With the increased number of multi-drug formulations, there is a need to develop new methods for simultaneous determinations of drugs. A precise, accurate and reliable liquid chromatographic method was developed for simultaneous determination of paracetamol, thiamine, and pyridoxal phosphate in pharmaceutical formulations. Separation of analytes was carried out with an Agilent Poroshell C18 column. A mixture of ammonium phosphate buffer (pH = 3.0), acetonitrile and methanol in the ratio of 86:7:7 (V/V/V) was used as the mobile phase pumped at a flow rate of 1.8 mL min−1. Detection of all three components, impurities and degradation products was performed at the selected wavelength of 270 nm. The developed method was validated in terms of linearity, specificity, precision, accuracy, LOD and LOQ as per ICH guidelines. Linearity of the developed method was found in the range 17.5–30 µg mL−1 for thiamine, 35–60 µg mL−1 for pyridoxal phosphate and 87.5–150 µg mL−1 for paracetamol. The coefficient of determination was ≥ 0.9981 for all three analytes. The proposed HPLC method was found to be simple and reliable for the routine simultaneous analysis of paracetamol, thiamine and pyridoxal phosphate in tablet formulations. Complete separation of analytes in the presence of degradation products indicated selectivity of the method.

Simultaneous determination of aflatoxin B1, aflatoxin B2, mycophenolic acid and sterigmatocystin in grape pomace by UHPLC-MS/MS

2014 ◽  
Vol 7 (2) ◽  
pp. 121-129 ◽  
Author(s):  
L. Luan ◽  
N. Chen ◽  
Z. Han ◽  
X. Liu ◽  
Y. Zheng ◽  
...  
Keyword(s):  
Simultaneous Determination ◽  
Mycophenolic Acid ◽  
Solid Phase ◽  
Multiple Reaction Monitoring ◽  
Reversed Phase ◽  
Grape Pomace ◽  
Relative Standard ◽  
Ultrahigh Performance Liquid Chromatography ◽  
Aflatoxin B

A reliable ultrahigh performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method was developed for the simultaneous determination of aflatoxin B1, aflatoxin B2, mycophenolic acid and sterigmatocystin in grape pomace. The samples were extracted by acetonitrile aqueous solution and further purified using a solid-phase extraction-based homemade clean-up cartridge. Next, the analytes were separated on a reversed-phase C18 column with a mobile phase consisting of water and acetonitrile. The separated compounds were detected with a tandem quadrupole mass spectrometer operating in positive electro-spray ionisation mode using multiple reaction monitoring. The established method was extensively validated by determining linearity (R2≯0.999), recovery (97.5-102.8%) and precision (relative standard deviation ≤7.0%). This method was then used for the simultaneous determination of the four mycotoxins in grape pomace samples.

scholarly journals Simultaneous Determination of Aspirin and Rosuvastatin Calcium in Capsules by Using RP-HPLC Coupled with Photo Diode Array Detection

2014 ◽  
Vol 33 ◽  
pp. 218-230
Author(s):  
Ankita Panchal ◽  
Gaurav Sanghvi ◽  
Ashish Vachhani ◽  
Navin Sheth ◽  
Devendra Vaishnav
Keyword(s):  
Quality Control ◽  
Simultaneous Determination ◽  
Lower Limit ◽  
Limit Of Detection ◽  
Pharmaceutical Formulations ◽  
Coefficient Of Determination ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
Rosuvastatin Calcium

A simple, sensitive, specific, and cost effective method for simultaneous determination of Aspirin and Rosuvastatin calcium was developed and validated in single dosage formulation. The sample solution of ASP and RSTC was prepared using methanol as a solvent. Separation of ASP and RSTC was achieved with a mobile phase consisting of 20 mM KH2PO4 : Methanol (30:70 v/v) at a flow rate of 1.0 ml/min. Separations were performed on Merck hibar 250-4.6 RP18 (5 µm) column (150 mm X 3.0 mm), using a Shimadzu Prominence HPLC system equipped with a Shimadzu SPD-20A detector, Rhenodyne 7725i injector with 20 μL loop, LC-20 AD pump, CBM-20 Alite controller and LC Solution software. Retention times of ASP and RSTC were 3.747 and 5.969 minutes respectively. Absolute recovery of ASP and RSTC was 100.3 and 100.03 % respectively. The lower limit of quantification (LLOQ) of ASP and RSTC was 0.3097 and 0.1063 ppm and lower limit of detection (LLOD) of ASP and RSTC was 0.01535 and 0.01358 ppm respectively. Linearity was established for the range of concentrations 15.00-90.0 μg/ml and 2.0-12.0 μg/ml for ASP and RSTC respectively with the coefficient of determination (R2) of 0.994 and 0.999 for both the compounds. The inter- and intra-day precision in the measurement of ASP quality control (QC) sample 75 μg/ml, were in the range 0.1-0.2 % relative standard deviation (R.S.D.) and 0.2-0.3 % R.S.D., respectively. The inter- and intra-day precision in the measurement of RST quality control (QC) sample 10 μg/ml, were in the range 0.1-0.2 % R.S.D., and 0.0-0.3 % R.S.D., respectively. The developed method would be applicable for routine quality control of ASP And RSTC in bulk as well as in pharmaceutical formulations

scholarly journals The RP-HPLC method development and validation for simultaneous determination of oryzalin and ethofumesate pesticides in soil and water

2021 ◽  
Author(s):  
Shishir Tandon ◽  
Suman Lata Pal
Keyword(s):  
Simultaneous Determination ◽  
Method Development ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Rp Hplc ◽  
Relative Standard ◽  
High Throughput Detection ◽  
Hplc Method Development ◽  
Soil And Water

Abstract A sensitive and reliable method for simultaneous determination of oryzalin and ethofumesate residues in pantnagar soil and water was validated. The compounds were extracted by LLE with dichloromethane from water, and acetone:methanol mixture from soil followed by SPE cleanup. Detection and quantification was done by RP-HPLC using mobile phase methanol:water (70:30, v/v) at 280 nm. The developed method showed satisfactory validation results with linearity (0.99), relative standard deviations (1.55 and 1.73%), and limit of quantification (0.002 μg g−1 and 0.005 μg g−1) for ethofumesate and oryzalin, respectively. Recoveries ranged for oryzalin and ethofumesate from 79.80–90.52, 75.58–86.04% (soil) and 83.50–95.92, 82.28–94.60% (water), respectively. The method could be used for routine high-throughput detection and determination of these compounds.

Simultaneous Determination of Ten Active Components in 12 Chinese Piper Species by HPLC

2011 ◽  
Vol 39 (05) ◽  
pp. 1043-1060 ◽  
Author(s):  
Cheng-Cheng Cai ◽  
Ma-Cheng Yan ◽  
Hui Xie ◽  
Sheng-Li Pan
Keyword(s):  
Simultaneous Determination ◽  
Correlation Coefficients ◽  
Current Method ◽  
Hplc Method ◽  
Central Nervous System Diseases ◽  
Hplc Separation ◽  
Active Components ◽  
Rp Hplc ◽  
Relative Standard

Piper is a genus that is recently valued for the treatment of central nervous system diseases. The major constituents, amides and lignans, are responsible for the antinociceptive and antidepressant activities. This study developed a RP-HPLC-UV method for the simultaneous determination of eight amides and two lignans in twelve different species of Piper. HPLC separation was accomplished on a C18 analytical column (5 μm, 250 mm × 4.6 mm, i.d.) with a gradient mobile phase consisting of acetonitrile and water at a flow rate of 1.0 ml/min. All the calibration curves showed good linear correlation coefficients (r > 0.9997) over the test ranges. The relative standard deviation of the current method was less than 2.90% for intra- and inter-day assays and the average recoveries were between 98.25% and 103.08%. The HPLC method established is appropriate for quality control purposes and allows for the differentiation of Piper species.

scholarly journals In Vitro Dissolution Study of Acetylsalicylic Acid and Clopidogrel Bisulfate Solid Dispersions: Validation of the RP-HPLC Method for Simultaneous Analysis

2020 ◽  
Vol 10 (14) ◽  
pp. 4792 ◽  
Author(s):  
Ehlimana Osmanović Omerdić ◽  
Larisa Alagić-Džambić ◽  
Marko Krstić ◽  
Maja Pašić-Kulenović ◽  
Jadranka Odović ◽  
...  
Keyword(s):  
Acetylsalicylic Acid ◽  
Simultaneous Determination ◽  
Solid Dispersions ◽  
Hplc Method ◽  
Poloxamer 407 ◽  
In Vitro Dissolution ◽  
Clopidogrel Bisulfate ◽  
Rp Hplc ◽  
Relative Standard

Solid dispersions were prepared via a solvent evaporation method, employing ethanol (96%, v/v) as solvent, with three different polymers as carrier: povidone, copovidone, and poloxamer 407. Previously developed reversed-phase HPLC (RP-HPLC) methods were modified and used for the simultaneous determination of acetylsalicylic acid and clopidogrel bisulfate and after release from solid dispersions. Chromatography was carried out on a C-18 column, with a mobile phase of acetonitrile–methanol–phosphate buffer pH 3.0, UV detection at 240 nm, and a run time of 6 min. The method was validated according to International Conference of Harmonisation guidelines and validation included specificity, accuracy, precision, linearity, robustness, limit of detection (LOD), and limit of quantification (LOQ). The method is specific for determination of acetylsalicylic acid and clopidogrel bisulfate. The linearity was provided in the concentration range 0.0275–0.1375 mg/mL for acetylsalicylic acid and 0.0200–0.1000 mg/mL for clopidogrel bisulfate, with a correlation coefficient (R2 value) of 0.9999 for both active pharmaceutical ingredients (APIs). Accuracy was confirmed by calculated recoveries for acetylsalicylic acid (98.6–101.0%) and clopidogrel bisulfate (100.0–101.6%). The intra-day and the inter-day precision-calculated relative standard deviations are less than 1%, which indicates high precision of the method. The limits of detection and quantification for acetylsalicylic acid were 0.0004 and 0.0012 mg/mL, and for clopidogrel bisulfate 0.0002 mg/mL and 0.0007 mg/mL, respectively. Small variations in chromatographic conditions did not significantly affect qualitative and quantitative system responses, which proved robustness of method. The proposed RP-HPLC method was applied for simultaneous determination of clopidogrel bisulfate and acetylsalicylic acid from solid dispersions.

scholarly journals Stability-indicating RP-HPLC assay for simultaneous determination of chlorpheniramine maleate and prednisolone in veterinary injection

2020 ◽  
Vol 32 (2) ◽  
pp. 122-127
Author(s):  
Amir Ali ◽  
Umar Farooq ◽  
Mahmood Ahmed ◽  
Muhammad Makshoof Athar ◽  
M. Salman ◽  
...  
Keyword(s):  
Simultaneous Determination ◽  
High Performance ◽  
Degradation Products ◽  
Hplc Method ◽  
Complete Separation ◽  
Calibration Graph ◽  
Coefficient Of Determination ◽  
Prednisolone Acetate ◽  
Chlorpheniramine Maleate

The present work described a simple, rapid, sensitive, accurate, and precise method for simultaneous determination of chlorpheniramine maleate (CHRM) and prednisolone acetate (PRED) in injection samples by high-performance liquid chromatography (HPLC) coupled with UV–Vis detection. Chromatographic separation was accomplished, employing isocratic mode and a mobile phase comprised of acetonitrile and a phosphate buffer (50:50, v/v, 30 °C), adjusted to pH 3.0. The flow rate used was 1.0 mL/min on a Thermo Hypersil ODS C18 column (5 μm, 4.6 × 250 mm), and the injection volume of sample was 20 μL. Analysis of CHRM and PRED was performed at a wavelength of 254 nm. The runtime for analysis was 12.5 min, and the retention times of CHRM and PRED were found to be 2.81 and 5.07 min, respectively. The calibration graph showed linearity over the concentration range 10–70 μg/mL for CHRM and 20–140 μg/mL for PRED with a coefficient of determination (R2) ≥0.9986. Repeatability and reproducibility (expressed as % RSD) were lower than 1.72 and 1.47%, respectively. The proposed HPLC method was demonstrated to be simple and rapid for the determination of CHRM and PRED in injection formulation, providing recoveries between 101.6–102.3%, whereas complete separation of degradation products, from analyte under investigation, provided the specificity of the proposed HPLC method.

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