Structural Elucidation of Potential Impurities in Azilsartan Bulk Drug by HPLC

2014 ◽  
Vol 97 (6) ◽  
pp. 1552-1562
Author(s):  
Wentao Zhou ◽  
Yuxia Zhou ◽  
Lili Sun ◽  
Qiaogen Zou ◽  
Ping Wei ◽  
...  
Keyword(s):  
Phosphoric Acid ◽  
Correlation Coefficient ◽  
Chromatographic Method ◽  
Hplc Method ◽  
Potassium Dihydrogen ◽  
The Mean ◽  
Bulk Drug ◽  
Potassium Dihydrogen Orthophosphate ◽  
Gradient Mode ◽  
Dihydrogen Orthophosphate

Abstract During the synthesis of Azilsartan (AZS), it was speculated that 15 potential impurities would arise. This study investigated the possible mechanism for the formation of 14 of them, and their structures were characterized and confirmed by IR, NMR, and MS techniques. In addition, an efficient chromatographic method was developed to separate and quantify these impurities, using an Inertsil ODS-3 column (250 × 4.6 mm, 5 μm) in gradient mode with a mixture of acetonitrile and the potassium dihydrogen orthophosphate buffer (10 mM, pH adjusted to 3.0 with phosphoric acid). The HPLC method was validated for specificity, precision, accuracy, and sensitivity. LOQ of impurities were in the range of 1.04–2.20 ng. Correlation coefficient values of linearity were >0.9996 for AZS and its impurities. The mean recoveries of all impurities in AZS were between 93.0 and 109.7%. Thus, the validated HPLC method is suitable for the separation and quantification of all potential impurities in AZS.

scholarly journals A Comparative Study of Newly Developed HPLC-DAD and UHPLC-UV Assays for the Determination of Posaconazole in Bulk Powder and Suspension Dosage Form

2014 ◽  
Vol 2014 ◽  
pp. 1-7 ◽  
Author(s):  
Dalia A. Hamdy ◽  
Tarek S. Belal
Keyword(s):  
Mobile Phase ◽  
Dosage Form ◽  
Gradient Elution ◽  
Potassium Dihydrogen ◽  
Bulk Powder ◽  
Ich Guidelines ◽  
The Mean ◽  
Potassium Dihydrogen Orthophosphate ◽  
Dihydrogen Orthophosphate

Objective. To develop and compare HPLC-DAD and UHPLC-UV assays for the quantitation of posaconazole in bulk powder and suspension dosage form.Methods. Posaconazole linearity range was 5–50 μg/mL for both assays. For HPLC-DAD assay, samples were injected through Zorbax SB-C18 (4.6 × 250 mm, 5 μm) column. The gradient elution composed of the mobile phase acetonitrile: 15 mM potassium dihydrogen orthophosphate (30 : 70 to 80 : 20, linear over 7 minutes) pumped at 1.5 mL/min. For UHPLC-UV assay, samples were injected through Kinetex-C18 (2.1 × 50 mm, 1.3 μm) column. The mobile phase composed of acetonitrile: 15 mM potassium dihydrogen orthophosphate (45 : 55) pumped isocratically at 0.4 mL/min. Detection wavelength was 262 nm in both methods.Results. The run time was 11 and 3 minutes for HPLC-DAD and UHPLC-UV assays, respectively. Both assays were linear (r2>0.999) with CV% and % error of the mean <3%. Limits of detection and quantitation were 0.82 and 2.73 μg/mL for HPLC-DAD and 1.04 and 3.16 μg/mL for UHPLC-UV, respectively. The methods quantitated PSZ in suspension dosage form with no observable interferences.Conclusions. Both assays were proven sensitive and selective according to ICH guidelines. UHPLC-UV assay exhibited some economic and chromatographic separation superiority.

DEVELOPMENT OF LIQUID CHROMATOGRAPHIC METHOD FOR ESTIMATION OF ACAMPROSATE CALCIUM AND BACLOFEN COMBINATION USED IN TREATMENT OF NEUROLOGICAL DISORDERS

INDIAN DRUGS ◽  
2021 ◽  
Vol 58 (03) ◽  
pp. 54-58
Author(s):  
Priyanka Jadeja ◽  
◽  
Jaimin S. Patel ◽  
Dimal A. Shah ◽  
Vandana B. Patel
Keyword(s):  
Neurological Disorders ◽  
Chromatographic Method ◽  
Potassium Dihydrogen ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic ◽  
Potassium Dihydrogen Orthophosphate ◽  
Isocratic Mode ◽  
Ich Guideline ◽  
Dihydrogen Orthophosphate

A specific, accurate, precise, and reproducible liquid chromatographic method has been developed and validated for the estimation of acamprosate calcium and baclofen in combination. The separation was achieved using stationary phase Phenomenex C18 column (150 mm× 4.6 mm.) in isocratic mode, with mobile phase containing 0.05 M potassium dihydrogen orthophosphate buffer (pH 7) : acetonitrile (10:90 V/V), at a flow rate of 1.0 mL/min and effluents were monitored at 210 nm. The retention time of acamprosate calcium and baclofen were found to be 1.9 min and 5.3 min, respectively. The linearity for acamprosate calcium and baclofen were in the range of 2-64 µg/mL and 1.2- 38.4 µg/mL, respectively. The method was validated as per ICH guideline. The recoveries of Acamprosate calcium and baclofen were found in the range of 98.90 - 100.13 % and 98.60 -100.02 %, respectively. The method was successfully applied for the determination of both the drugs in combination.

A Versatile Stability-indicating Liquid Chromatographic Method for the Simultaneous Determination of Atenolol, Hydrochlorothiazide and Chlorthalidone

2020 ◽  
Vol 16 (8) ◽  
pp. 1037-1051
Author(s):  
Ehab Farouk Elkady ◽  
Marwa Ahmed Fouad ◽  
Abdulgabar A. Ezzy Faquih
Keyword(s):  
Quality Control ◽  
Chromatographic Method ◽  
Degradation Products ◽  
Pharmaceutical Dosage Forms ◽  
Potassium Dihydrogen ◽  
Ich Guidelines ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic ◽  
Potassium Dihydrogen Orthophosphate

Background: Atenolol is a selective beta 1 blocker that can be used alone or in combination with hydrochlorothiazide or with chlorthalidone for the treatment of hypertension and prevention from a heart attack. Objective: The main target of this work was to improve modern, easy, accurate and selective liquid chromatographic method (RP-HPLC) for the determination of these drugs in the presence of their degradation products. These methods can be used as analytical gadgets in quality control laboratories for a routine examination. Methods: In this method, the separation was accomplished through an Inertsil® ODS-3V C18 column (250 mm x 4.6 mm, 5 μm), the mobile phase used was 25 mM aqueous potassium dihydrogen orthophosphate solution adjusted to pH 6.8 by using 0.1M sodium hydroxide and acetonitrile (77 : 23, v/v), the flow rate used was 1 ml/min and detection was achieved at 235 nm using UV. Results: All peaks were sharp and well separated, the retention times were atenolol degradation (ATN Deg.) 2.311 min, atenolol (ATN) 2.580 min, hydrochlorothiazide degradation (HCT Deg.) 5.890 min, hydrochlorothiazide (HCT) 7.016 min, chlorthalidone degradation CTD Deg 8.018 min and chlorthalidone (CTD) 14.972 min. Linearity was obtained and the range of concentrations was 20- 160 μg/ml for atenolol, 10-80 μg/ml for hydrochlorothiazide and 10-80 μg/ml for chlorthalidone. According to ICH guidelines, method validation was accomplished, these methods include linearity, accuracy, selectivity, precision and robustness. Conclusion: The optimized method demonstrated to be specific, robust and accurate for the quality control of the cited drugs in pharmaceutical dosage forms.

scholarly journals Validated High-Throughput HPLC Method for the Analysis of Flavonol Aglycones Myricetin, Quercetin, and Kaempferol in Rhus coriaria L. Using a Monolithic Column

2009 ◽  
Vol 92 (4) ◽  
pp. 1035-1043 ◽  
Author(s):  
Morteza Mehrdad ◽  
Mahnoosh Zebardast ◽  
Ghazaleh Abedi ◽  
Mitra Nouri Koupaei ◽  
Hoda Rasouli ◽  
...  
Keyword(s):  
High Performance ◽  
Monolithic Column ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Hplc Method ◽  
Potassium Dihydrogen ◽  
Liquid Chromatographic Method ◽  
Rhus Coriaria ◽  
Liquid Chromatographic ◽  
Potassium Dihydrogen Orthophosphate

Abstract A rapid and simple reversed-phase high-performance liquid chromatographic method using a monolithic column was developed and validated for the separation and quantification of myricetin, quercetin, and kaempferol in Rhus coriaria L. The method employed the isocratic mobile phase acetonitrile10 mM potassium dihydrogen orthophosphate buffer adjusted to pH 3.0 using orthophosphoric acid (38 + 62, v/v) at a flow rate of 4.0 mL/min; a Chromolith Performance RP-18e (100 4.6 mm) monolithic column kept at 40C; and UV detection at 370 nm. Although the elution order was identical and the selectivity was equivalent, the comparison between monolithic and particulate columns showed that the monolithic column could reduce the separation time to &lt;1 min without sacrificing column efficiency and selectivity. The method was validated according to International Conference on Harmonization guidelines. The validation characteristics included accuracy, precision, linearity, range, specificity, LOQ, and robustness. The calibration curves were linear (r &gt;0.999) over the concentration range of 0.8888.3 g/mL for myricetin, 0.9595 g/mL for quercetin, and 1.43143.3 g/mL for kaempferol. The recoveries for all three compounds were above 89. Myricetin was found to be the major flavonol in the examined plant extracts, followed by minor quantities of quercetin and kaempferol.

Nucleation in supersaturated potassium dihydrogen orthophosphate solutions

1979 ◽  
Vol 46 (1) ◽  
pp. 7-9 ◽  
Author(s):  
M.S. Joshi ◽  
A.V. Antony
Keyword(s):  
Potassium Dihydrogen ◽  
Potassium Dihydrogen Orthophosphate ◽  
Dihydrogen Orthophosphate

scholarly journals HPLC Quantitative Analysis of Main Stilbenes and Flavones in Different Parts ofMatteuccia struthiopteris

2013 ◽  
Vol 2013 ◽  
pp. 1-6 ◽  
Author(s):  
Shubei Li ◽  
Dong Zhang ◽  
Lan Yang ◽  
Yujie Li ◽  
Xiaoxin Zhu ◽  
...  
Keyword(s):  
Quantitative Analysis ◽  
Linear Regression ◽  
Phosphoric Acid ◽  
Flow Rate ◽  
Mobile Phase ◽  
Gradient Elution ◽  
Hplc Method ◽  
Regression Coefficients ◽  
The Mean ◽  
Different Parts

A simple and accurate HPLC-UV method was developed for the simultaneous quantitative analysis of main stilbenes and flavones in different parts (fronds, rhizomes, and frond bases) ofM. struthiopteris. The chromatographic separation was performed on a Kromasil C18 column (4.6 mm × 250 mm, 5 μm) with the mobile phase of MeOH-H2O (including 0.1% phosphoric acid) using a gradient elution at the flow rate of 1.0 mL min−1and UV detection at 295 nm. The method was validated by specificity, linearity, accuracy (recovery), and precision tests (repeatability, intra- and interday). For all the six compounds, the linear regression coefficients ranged from 0.9958 to 0.9998 within the test ranges; intra- and interday precisions were<2% and the mean recoveries ranged from 98.09 to 103.56%. The amount of these compounds in the frond bases was almost the same as in the rhizomes but much higher than that in the fronds. The results indicate that the HPLC method developed was appropriate for the analysis of the six compounds in different parts (fronds, rhizomes, and frond bases) ofM. struthiopteris.

Transport properties and modification of potassium dihydrogen orthophosphate

2016 ◽  
Vol 52 (12) ◽  
pp. 1276-1282
Author(s):  
I. N. Bagryantseva ◽  
V. G. Ponomareva
Keyword(s):  
Transport Properties ◽  
Potassium Dihydrogen ◽  
Potassium Dihydrogen Orthophosphate ◽  
Dihydrogen Orthophosphate

Nucleation studies in supersaturated potassium dihydrogen orthophosphate solution and the effect of soluble impurities

1984 ◽  
Vol 19 (9) ◽  
pp. 2837-2844 ◽  
Author(s):  
M. Shanmugham ◽  
F. D. Gnanam ◽  
P. Ramasamy
Keyword(s):  
Potassium Dihydrogen ◽  
Potassium Dihydrogen Orthophosphate ◽  
Dihydrogen Orthophosphate

Effects of fertilizer on concentrations of copper, molybdenum, and sulfur in subterrranean clover (Trifolium subterraneum)

1981 ◽  
Vol 21 (112) ◽  
pp. 491 ◽  
Author(s):  
GD Reddy ◽  
AM Alston ◽  
KG Tiller
Keyword(s):  
Animal Health ◽  
Sodium Molybdate ◽  
Subterranean Clover ◽  
Trifolium Subterraneum ◽  
Dry Weight ◽  
Calcareous Sand ◽  
Potassium Dihydrogen ◽  
Podzolic Soils ◽  
Potassium Dihydrogen Orthophosphate ◽  
Dihydrogen Orthophosphate

In pot experiments, subterranean clover (Trifolium subterraneum) was grown on four soils; two lateritic podzolic soils, a red-brown earth and a calcareous sand, to which various combinations of phosphorus (0 to 45 ppm as potassium dihydrogen orthophosphate), sulfur (0 to 45 ppm as calcium sulfate), copper (0 to 10 ppm as copper sulphate) and molybdenum (0 to 1 ppm as sodium molybdate) had been added. Applications of sulfur and copper had little effect on the dry weight of the clover tops on any soil, and none of the fertilizers affected dry weight on the calcareous sand. On the other soils, dry weight was increased by phosphorus, and by molybdenum when applied in combination with phosphorus. The copper treatment consistently increased the concentration of that element in the tops of the plants. On the lateritic podzolic soils and the red-brown earth, sulfur generally increased copper and sulfur concentrations but decreased that of molybdenum; phosphorus decreased copper and sulfur but increased the concentration of molybdenum. On the calcareous sand, application of sulfur had no effect on copper but decreased molybdenum and increased sulfur concentration; treatment with phosphorus decreased the concentration of copper but had no effect on sulfur or molybdenum in the plant tops. There were significant interactions between all treatments. These are discussed in relation to fertilizer practice and animal health.

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