Trace Level Quantification of the (−)2-(2-amino-5-chlorophenyl)-4-cyclopropyl-1,1,1-trifluoro-3-butyn-2-ol Genotoxic Impurity in Efavirenz Drug Substance and Drug Product Using LC–MS/MS

Jaishetty, Nagadeep; Kamaraj, P.; Maruthapillai, Arthanareeswari; Jaishetty, Rajamanohar

doi:10.3390/scipharm84030456

Cited by 12 publications

(8 citation statements)

References 15 publications

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“…The aim of the present article describes the quantitative determination of (S)-enantiomer of sitagliptin phosphate in a combination dosage of SIT and MET by using reverse phase chromatography. In continuation of our research work for determination of impurities in pharmaceutical dosage forms [22][23], the present communication forms the first report of a simple, sensitive and reproducible method for determination of (S)-enantiomer of sitagliptin phosphate in combination product of SIT and MET.…”

Section: Introductionmentioning

confidence: 82%

Enantiometric Separation of Sitagliptin in a Fixed Dose Combination Formula of Sitagliptin and Metformin by a Chiral Liquid Chromatographic Method

Jaishetty

Kamaraj

Maruthapillai

2019

Int J Pharm Pharm Sci

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Objective: Sitagliptin phosphate and metformin hydrochloride tablet is an FDA approved combination product for the treatment of diabetes mellitus type 2. There are no reported evidence for estimation of undesired (S)-sitagliptin in a combination product. The objective of this study was to develop a high sensitive liquid chromatography method for the determination of (S)-enantiomer of sitagliptin phosphate in a fixed dose combination formula of metformin and sitagliptin. Methods:The proposed novel high-performance liquid chromatography (HPLC) method uses programmed gradient elution of a mixture of ethanoldiethylamine(DEA) 100:0.1 (v/v) as mobile phase-A and a mixture of methanol-water 60:40 (v/v) as mobile phase-B. The chromatographic conditions were designed to nullify the metformin interference and in which sitagliptin enantiomers elute first and followed by metformin. A satisfactory resolution (≥2.5) between (S) -sitagliptin and active form (R)-sitagliptin was achieved with gradient elution on Chiralpak IA column (5μm, 4 × 250 mm) at a flow rate of 0.5 ml/min and the detector wavelength set at 265 nm. The injection volume set as 10 µl. The developed method has been validated as per the International Conference on Harmonisation (ICH) guidelines. Results:The proposed HPLC method for determination of (S)-sitagliptin, showed good linearity in the concentration range of 0.5 µg/ml to 13.6 µg/ml and capable to quantify accurately up to the lowest level (LOQ) of 0.017%. The validated method was successfully applied to quantify the (S)sitagliptin for different marketed formulations of sitagliptin with metformin and sitagliptin alone, and the corresponding recovery values were found to be in the range of 95.1% to 98.4%. Conclusion:The proposed validated HPLC method was found to be suitable for the quantitative determination of (S)-sitagliptin in the formulations of sitagliptin with metformin and sitagliptin alone.

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Section: Introductionmentioning

confidence: 82%

Enantiometric Separation of Sitagliptin in a Fixed Dose Combination Formula of Sitagliptin and Metformin by a Chiral Liquid Chromatographic Method

Jaishetty

Kamaraj

Maruthapillai

2019

Int J Pharm Pharm Sci

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“…To determined impurities, LC-MS/MS methods had been reported for trace level determination of AMCOL, which was a process-related impurity and degradation impurity of efavirenz also determined (Fig. 24) [47].…”

Section: Efavirenzmentioning

confidence: 99%

Genotoxic Impurities: An Important Regulatory Aspect

Pounikar

Umekar

Gupta

2020

Asian J Pharm Clin Res

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Genotoxins are agents/carriers such as chemical or radiation that can cause the damage to DNA or chromosomal structure, thereby causing mutations and the process are called as genotoxicity. Identification and understanding of genotoxins at a primary stage of drug development would enable us to prevent the potential damage that can be caused by these genotoxic agents. Various regulatory agencies such as International Council for Harmonization and EMEA, USFDA, European Pharmacopeia guidance, guidance for oncology products provide guidelines to limits the level of impurities in drug substances and drug products. Nowadays, conventional protocol of isolation, various spectral analysis high-performance liquid chromatography (LC), Fourier transform infrared to on-line analysis using modern, sophisticated hyphenated tools, like gas chromatography-mass spectroscopy, LC-MS so on, as well as modern software based in silico drug designs are extensively used by industry, research, and development areas and also there is tremendous increase in publications in the literature involving their use. Our review article focused on the various regulatory guidelines, application of hyphenated tools, and in silico techniques in genotoxic impurity and degradation product profiling of small molecules. A brief explanation is made on possible pitfalls in the experimentation and data interpretation. From this review, it concluded that there are various countries having their own regulatory agencies and regulatory guidelines for drug approvals, which may be followed by applying new chemical entities the new drug application title (NDA) in new drug application as well as there are various conventional to modern software based techniques to quantification of genotoxic impurities.

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“…Avaram Senna (Cassia auriculata linn), commonly known as Tanner's Cassia is wild and perennial plant. Cassia species are well known for their laxative, purgative constituents and used for skin diseases [9]. Neem is a life-giving tree, especially in the arid coastal and southern areas, and it is used medicinally as an antibiotic, antiseptic, and to treat head lice.…”

Section: Introductionmentioning

confidence: 99%

Studies on Poly Herbal Powder Shampoo for the Treatment of Pediculosis Capitis and Pityriasis Capitis Infestations

MOHAMED¹,

Elhassan

Khan

et al. 2022

Int J App Pharm

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Objective: The main objective of this study was to the formulation containing polyherbal medicinal plants, which gives safety, and efficacy; rectify skin disease, scalp disorders and reducing the harmful effect from herbal anti-lice and dandruff shampoos for the treatment of Pediculosis capitis and Pityriasis capitis and to prevent hair fall. Methods: The formulation of herbal shampoo with various herbal ingredients were dried, milled, sieved (120#) and mixed in geometrical order and evaluated their physicochemical characteristics. Furthermore, particle characters, organoleptic properties, foaming index, skin irritation study, and Anti-lice activity were performed. Results: The prepared poly herbal powdered shampoo (PHPS) exhibits that was freely soluble, particle 20-25 μm size range and free-flowing powder. Lest moisture content (2.5%), ash value, acid value and reduced surface tension of liquid are referred as an ideal candidate for foaming, anti-lice potential with no skin irritations. Conclusion: Based on the evaluation parameters, the prepared powdered shampoo helps to remove hair grease, no hair fall and strengthen hair follicles. Preparation of PHPS formulation at laboratory scale and the compounding of several ingredients of herbal source have produced it possible to ensure safety, efficacy and secure highly effective PHPS.

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Trace Level Quantification of the (−)2-(2-amino-5-chlorophenyl)-4-cyclopropyl-1,1,1-trifluoro-3-butyn-2-ol Genotoxic Impurity in Efavirenz Drug Substance and Drug Product Using LC–MS/MS

Cited by 12 publications

References 15 publications

Enantiometric Separation of Sitagliptin in a Fixed Dose Combination Formula of Sitagliptin and Metformin by a Chiral Liquid Chromatographic Method

Enantiometric Separation of Sitagliptin in a Fixed Dose Combination Formula of Sitagliptin and Metformin by a Chiral Liquid Chromatographic Method

Genotoxic Impurities: An Important Regulatory Aspect

Studies on Poly Herbal Powder Shampoo for the Treatment of Pediculosis Capitis and Pityriasis Capitis Infestations

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