Chiral separation of sitagliptin phosphate enantiomer by HPLC using amylose based chiral stationary phase

Reddy, Bhimireddy Venkata Rami; Raman, N.V.V.S.S.; Kumar, B.sai; Rambabu, C.

doi:10.1016/j.jopr.2013.06.014

Cited by 11 publications

(2 citation statements)

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“…The retention times of the optimized method on chiral cell OD-RH column were found to be 4.06 & 4.66 min., which is better in comparison to the work carried out with amylose-based chiral stationary phase. [31,35] The method separated sitagliptin's (S) and (R) enantiomers in rat serum. The concentration of organic modifier (ACN) and buffer strength (Borax) played an important role in achieving better retention and resolution between the enantiomers of sitagliptin.…”

Section: Discussionmentioning

confidence: 99%

“…The interaction is through hydrogen bonding between C=O and NH group present in the CSP with C=O and OH group in the STG drug molecule. [30,31] Hence, to the best of our knowledge, no chiral LC method by direct analysis of sitagliptin (STG) enantiomers in rat serum has been reported so far in the literature. Hence, this study was undertaken.…”

Section: Abstract a R T I C L E I N F Omentioning

confidence: 99%

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Enantioselective RP-UFLC Method for the Simultaneous Estimation of Sitagliptin (STG) enantiomers (R and S) in racemic mixture and their Pharmacokinetic assessment in male Wistar Rats

Veeresham

Srinivas

Qureshi

et al. 2022

Int. J. Pharm. Sci. Drug Res.

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The present work aims to develop and validate a simple, rapid, and reproducible reverse phase ultra-fast liquid chromatography method with a UV detector (RP-UFLC-UV) was developed for the separation and determination of sitagliptin (STG) enantiomers (S-(STG) and R-(STG)) simultaneously. Baseline separation was achieved on Lux cellulose-1 column, (cellulose tri-(3,5-dimethyl phenyl carbamate (Chiralcel OD-RH, 250 mm × 4.6 mm, 5 µm) column and mobile phase consisted of 20mM borate buffer solution (pH = 9±0.05) and ACN in the ratio of (60:40, v/v) at a flow rate of 0.8 mL/min was used. Detection of peaks was monitored at 262 nm. For analyzing the STG enantiomers in the rat serum and pure API, a method was developed using the chiral RP-UFLC-UV method was validated. The single oral dose of 2.5 mg/kg of STG racemate was administered to a group of 6 healthy rats for a comparative pharmacokinetic study of both the enantiomers. The linear range of the calibration curve for each enantiomer was 0.5–64 µg/mL. The precision of this method at concentrations between 0.5–48 µg/mL was within 8.65% and the % recovery (accuracy) of both sitagliptin (STG) enantiomers (S-(STG) and R-(STG) were 98.47–101.02% and 98.93- 100.52%. The precision at LLOQ (0.5 µg/mL) was between 8.65%-7.09%, which was poor than that at QC levels, and the average extraction recovery was higher than 85% for both sitagliptin (SGT) enantiomers at QC levels, and its pharmacokinetics of enantiomers was found to be stereoselective.

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Section: Discussionmentioning

confidence: 99%

Section: Abstract a R T I C L E I N F Omentioning

confidence: 99%

Enantioselective RP-UFLC Method for the Simultaneous Estimation of Sitagliptin (STG) enantiomers (R and S) in racemic mixture and their Pharmacokinetic assessment in male Wistar Rats

Veeresham

Srinivas

Qureshi

et al. 2022

Int. J. Pharm. Sci. Drug Res.

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Environmentally friendly protocol for the determination of sitagliptin phosphate in pharmaceutical preparations and biological fluids using l‐tyrosine as a fluorescence probe

2023

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A responsive spectrofluorimetric method was developed for the determination of sitagliptin phosphate using L‐tyrosine as a fluorescence probe. The fluorescence intensity of L‐tyrosine was quenched with sitagliptin phosphate. The fluorescence intensity was recorded at 307 nm using a 272 nm excitation wavelength. The calibration plot between fluorescence intensity and the concentration of drug was liner in the range of 0.1 to 2.0 mM with a good correlation value of 0.997. The limit of detection and quantification were established to be 3.7 × 10‐4 and 1.23 × 10‐3 mM, respectively. Commonly used excipients did not interfere with sitagliptin phosphate measurement. The proposed method was used to measure the sitagliptin phosphate in its standard type, dosage form, and biological samples. The percent recovery were ranged from 97.41–103.36 %. The static quenching was shown to be responsible for quenching as indicated by the Stern–Volmer plot. The method was validated usin ICH guidelines and profitably applied for the content uniformity test, ensuing in a high percent recovery and small relative standard deviation. The proposed approach is effortless, susceptible, selective, economic, and provides a high precision and accuracy, and can be used to determine sitagliptin phosphate in pharmaceutical industry.

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A concise review of the bioanalytical methods for the quantitation of sitagliptin, an important dipeptidyl peptidase‐4 (DPP4) inhibitor, utilized for the characterization of the drug

Suresh

Srinivas²,

Mullangi

2016

Biomedical Chromatography

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Inhibition of dipeptidyl peptidase-4 (DPP4) is an emerging therapeutic approach for treating type 2 diabetes and has revolutionized the concept of diabetes management. Sitagliptin is the first approved orally active, potent, selective and nonpeptidomimetic DPP4 inhibitor. Incidence of hypoglycemia and weight gain is negligible with sitagliptin treatment. It is used as monotherapy or in combination with other anti-diabetic drugs to treat type 2 diabetes. There are numerous bioanalytical methods published for the analysis of sitagliptin in preclinical and clinical samples. This review focuses on the various HPLC and LC-MS/MS methods that have been used to analyze sitagliptin in various biological matrices. A small section is devoted to the bioanalysis of other DPP4 inhibitors such as vildagliptin, saxagliptin and linagliptin. This review provides key information in a concise manner regarding sample processing options, chromatographic/detection conditions and validation parameters of the chosen methods for sitagliptin and other DPP4 inhibitors.

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Chiral separation of sitagliptin phosphate enantiomer by HPLC using amylose based chiral stationary phase

Cited by 11 publications

References 1 publication

Enantioselective RP-UFLC Method for the Simultaneous Estimation of Sitagliptin (STG) enantiomers (R and S) in racemic mixture and their Pharmacokinetic assessment in male Wistar Rats

Enantioselective RP-UFLC Method for the Simultaneous Estimation of Sitagliptin (STG) enantiomers (R and S) in racemic mixture and their Pharmacokinetic assessment in male Wistar Rats

Environmentally friendly protocol for the determination of sitagliptin phosphate in pharmaceutical preparations and biological fluids using l‐tyrosine as a fluorescence probe

A concise review of the bioanalytical methods for the quantitation of sitagliptin, an important dipeptidyl peptidase‐4 (DPP4) inhibitor, utilized for the characterization of the drug

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