Chiral HPLC Separation, Absolute Structural Elucidation, and Determination of Stereochemical Stability oftrans-Bis[2-(2-pyridinyl)aminophenolato] Cyclotriphosphazene

Chirality ◽  
2016 ◽  
Vol 28 (7) ◽  
pp. 556-561 ◽  
Author(s):  
Kazumasa Kajiyama ◽  
Yuki Setone ◽  
Kouki Aoyagi ◽  
Hidetaka Yuge
Keyword(s):  
Structural Elucidation ◽  
Chiral Hplc ◽  
Hplc Separation

A Validated Chiral HPLC Method for the Enantiomeric Separation of Melphalan HCl

2013 ◽  
Vol 781-784 ◽  
pp. 993-998
Author(s):  
Li Ping Gao ◽  
Wen Juan Li ◽  
Xin Ping Wang
Keyword(s):  
Perchloric Acid ◽  
Mobile Phase ◽  
Enantiomeric Separation ◽  
Hplc Method ◽  
Chiral Hplc ◽  
Hplc Separation ◽  
Perchloric Acid Solution ◽  
Anti Cancer ◽  
Chromatographic Resolution

A new and accurate chiral HPLC method was developed for the determination of Melphalan HCl, L-Phenylalanine, 4-bis (2-chloroethyl) amino hydrochloride an anti-cancer chemotherapy drug and its potential impurity namely D-Phenylalanine, 4-bis (2-chloroethyl) amino hydrochloride ( D-enantiomer) in bulk substance. HPLC separation was carried out by reverse phase chromatography on Crownpak CR (+) (5μm, 4.0x150mm) with a mobile phase composed of perchloric acid (pH 4.0): methanol in the ratio of 90:10. Melphalan and its potential impurities were baseline resolved in the optimized method. The pH of perchloric acid solution in the mobile phase has played a key role in achieving chromatographic resolution between the enantiomers and in enhancing chromatographic efficiency. The developed method was completely validated and proved to be robust. The validated method yielded good results regarding specificity, precision, linearity, accuracy, robustness, sensitivity. Melphalan HCl sample solution is found to be stable for at least 60hrs at room temperature. The proposed method was found to be suitable and accurate for quantitative determination of Melphalan HCl and its D-enantiomer in bulk substance.

Determination of process-related impurities in N-acetylglucosamine prepared by chemical and enzymatic methods: structural elucidation and quantification

2016 ◽  
Vol 39 (7) ◽  
pp. 937-945
Author(s):  
Yi Soo Kim ◽  
Sung Joong Lee ◽  
Jin Young Choi ◽  
Yun-Hi Kim ◽  
Kebede Taye Desta ◽  
...  
Keyword(s):  
Structural Elucidation ◽  
Related Impurities ◽  
Enzymatic Methods

scholarly journals Validation of developed method by RP-HPLC for simultaneous estimation of famotidine and ibuprofen in human plasma and studying the stability of the drugs in plasma

2018 ◽  
Vol 12 (1) ◽  
pp. 34-48
Author(s):  
K. S Ashutosh ◽  
D. Manidipa ◽  
R. J. V. L. N. Seshagiri ◽  
S. D. Gowri
Keyword(s):  
Human Plasma ◽  
Mobile Phase ◽  
Simultaneous Estimation ◽  
Hplc Separation ◽  
Reverse Phase ◽  
Rp Hplc ◽  
The Stability ◽  
Sodium Dihydrogen ◽  
Isocratic Mode

The RP-HPLC separation was carried out by reverse phase chromatography on a Symmetry C18 (4.6 x 150 mm, 3.5 μm, make: XTerra) with a mobile phase composed of sodium dihydrogen ortho phosphate [pH 2.5] and acetonitrile in the ratio of 30:70 v/v in an isocratic mode at a flow rate of 1.2 mL/min. The run time was maintained for 8.0 min. The detection was monitored at 236 nm. The accuracy was calculated in human plasma and the % recovery was found 99.80 - 99.85 for famotidine and 99.56 -99.85.5 for ibuprofen and reproducibility was found to be satisfactory. The calibration curve for famotidine in human plasma was linear over 3.32 to 6.65 μg/mL and 100- 200 μg/mL for ibuprofen in human plasma respectively. The inter-day and intra-day precision in human plasma was found within limits. The proposed method has adequate sensitivity, reproducibility, and specificity for the determination of famotidine and ibuprofen in plasma. The LLOQ obtained by the proposed method in human plasma were 1.24 and 5.0 μg/mL for famotidine and ibuprofen respectively. The proposed method is simple, fast, accurate, and precise for the quantification of famotidine and ibuprofen in plasma as per the ICH guidelines.Kathmandu University Journal of Science, Engineering and TechnologyVol. 12, No. I, June, 2016, Page: 34-48

scholarly journals HPLC determination of hydrochlorothiazide in urine after solid-phase extraction

2005 ◽  
Vol 51 ◽  
pp. 23-28 ◽  
Author(s):  
Violeta Ivanova ◽  
Dragica Zendelovska ◽  
Marina Stefova
Keyword(s):  
Particle Size ◽  
Solid Phase Extraction ◽  
Mobile Phase ◽  
Solid Phase ◽  
Hplc Method ◽  
Phase Extraction ◽  
Hplc Separation ◽  
Isocratic Elution ◽  
Extraction Recovery

A simple, rapid and precise HPLC method has been developed for the assay of hydrochlorothiazide in urine. The clean-up of the urine samples was carried out by solid-phase extraction using HLB cartridges. Extraction recovery was 94.00-100.28 %. HPLC separation was performed with isocratic elution on Hypersil BDS C18 column (100 x 4.0 mm I.D., 3 µm particle size) protected with appropriate guard column. The mobile phase was 18 % acetonitrile and 0.025 mol/L solution of KH2PO4, pH 4 at flow rate of 0.3 mL/min. Detection of the substances was performed at 220 nm. The calibration curves were linear in the range of 2-50 µg/mL. The developed method is validated by checking its accuracy, precision and stability. The detection limit is 2 µg/mL hydrochlorothiazide. The method is proved to be convenient for routine analysis of hydrochlorothiazide in urine.

The determination of enantiomer composition of 1-((3-chlorophenyl)-(phenyl)methyl) amine and 1-((3-chlorophenyl)(phenyl)-methyl) urea (Galodif) by NMR spectroscopy, chiral HPLC, and polarimetry

Chirality ◽  
2018 ◽  
Vol 30 (10) ◽  
pp. 1135-1143
Author(s):  
Vera Yu. Kuksenok ◽  
Victoria V. Shtrykova ◽  
Victor D. Filimonov ◽  
Alexandr G. Druganov ◽  
Alexandr A. Bondarev ◽  
...  
Keyword(s):  
Nmr Spectroscopy ◽  
Chiral Hplc ◽  
Methyl Amine ◽  
Enantiomer Composition

scholarly journals Reverse Phase Chiral HPLC Method for Enantiomeric Excess Determination of 2-Aminobutanamide

2019 ◽  
Vol 32 (1) ◽  
pp. 69-72
Author(s):  
T. Naga Jhansi ◽  
D. Pavan Kumar ◽  
Nagaraju Rajana ◽  
D. Jayadeep Kumar ◽  
G. Nageswara Rao
Keyword(s):  
Limit Of Detection ◽  
Enantiomeric Excess ◽  
Hplc Method ◽  
Chiral Hplc ◽  
Reverse Phase ◽  
Limit Of Quantification ◽  
Perchloric Acid Solution ◽  
Column Temperature ◽  
Isomer Content

A reverse phase chiral HPLC method was developed for the determination of (R)-2-aminobutanamide isomer content in (S)-2-amino-butanamide key starting material for levetiracetam drug substance by using a CROWNPAK CR (+) column. Perchloric acid solution (0.05 %) was used as mobile phase and the flow rate was finalized as 0.3 mL/min. UV detection wavelength was 200 nm and column temperature was set as 15 ºC. The limit of detection and limit of quantification were 0.0002 mg/mL and 0.0005 mg/mL, respectively. The linearity calibration curve of (R)-2-aminobutanamide was shown good from the range of 0.0005 mg/mL to 0.004 mg/mL. The recovery of (R)-2-aminobutanamide isomer was between the range of 93 to 106 % in presence of (S)-2-aminobutanamide. The method was validated and found to be precise, accurate and robust. The method can be used for determination of (R)-2-aminobutanamide in presence of (S)-2-aminobutanamide, which is the key intermediate for preparation of levetiracetam. This method was validated in as per ICH Q2 (R1) and USP validation of compendial methods (1225).

A Validated Chiral HPLC Method for the Determination of Enantiomeric Purity of R-β-amino-β-(4-methoxyphenyl) Propionic Acid

2006 ◽  
Vol 65 (1-2) ◽  
pp. 81-84 ◽  
Author(s):  
P. Madhavan ◽  
B. M. Rao ◽  
Pravin ◽  
Abhishek ◽  
P. R. Kumar ◽  
...  
Keyword(s):  
Propionic Acid ◽  
Hplc Method ◽  
Enantiomeric Purity ◽  
Chiral Hplc
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