A Novel RP-HPLC Method for Estimating Fulvestrant, Benzoyl Alcohol, and Benzyl Benzoate in Injection Formulation

Nekkalapudi, Arjuna Rao; Veldi, Venu Gopal; Pippalla, Sreenivas

doi:10.4236/ajac.2022.137016

Cited by 11 publications

(5 citation statements)

References 14 publications

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“…(S)-1-(4-(4-amino-4-(1H-benzo[d]imidazol-2-yl)butyl) guanidine (IVa) is obtained as a gray powder. For analytical purposes, the product (IVa) is additionally was purified by prep-HPLC (Phenomenex Luna C18 100 mm × 40 mm × 5 μm, 70 mobile phase: [water (0.1%TClA) − ACN]: 20−55%, 12 min).1H-NMR (400 MHz, DMSO-d6): δ 1.50 (m, 2H), 1.81 (m, 2H), 2.52 (s, 1H), 3.33 (m, 2H),3.8 (s, 1H), 7.16 (d,1H), 7.52 (s, 1H), 8.76 (s, 2H), 6.63 (s, 2H), 7.82 (s, 1H), 12.16 (s, 1H). 13CNMR (126 MHz, CD 3 OD) δ 24.39, 25.70, 30.66, 43.07, 58.05, 58.66, 79.19, 100.37.…”

Section: Methodsmentioning

confidence: 99%

“…(S)-1-(4-(4-amino-4-(1H-benzo[d]imidazol-2-yl)butyl) guanidine (IVa) is obtained as a gray powder. For analytical purposes, the product (IVa) is additionally was purified by prep-HPLC (Phenomenex Luna C18 100 mm × 40 mm × 5 μm, 70 Histidine (155 mg, 1.0 mmol) and benzene-1,2-diamine (108 mg, 1.0 mmol), dissolve in 5 mL anhydrous glacial acetic acid (AGAA) in a 20 mL round bottom flask, place in a system with a reflux condenser and a Dean-Stark nozzle. Boil with the reflux condenser and extract 3 mL of AGAA.…”

Section: Materials and Equipmentmentioning

confidence: 99%

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Molecular Modeling, Synthesis, and Antihyperglycemic Activity of the New Benzimidazole Derivatives – Imidazoline Receptor Agonists

Martynov,

Farber,

Bomko

et al. 2024

DDDT

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Introduction The paper presents the results of a study on the first synthesized benzimidazole derivatives obtained from labile nature carboxylic acids. The synthesis conditions of these substances were studied, their structure was proved, and some components were found to have sugar-reducing activity on the model of alloxan diabetes in rats. Methods The study used molecular modeling methods such as docking based on the evolutionary model (igemdock), RP_HPLC method to monitor the synthesis reaction, and 1H NMR and 13C NMR, and other methods of organic chemistry to confirm the structures of synthesized substances. Results & Discussion The docking showed that the ursodeoxycholic acid benzimidazole derivatives have high tropics to all imidazoline receptor carriers (PDB ID: 2XCG, 2bk3, 3p0c, 1QH4). The ursodeoxycholic acid benzimidazole derivative and arginine and histidine benzimidazole derivatives showed the highest sugar-lowering activity in the experiment on alloxan-diabetic rats. For these derivatives, the difference in glucose levels of treated rats was significant against untreated control. Therefore, the new derivatives of benzimidazole and labile natural organic acids can be used to create new classes of imidazoline receptor inhibitors for the treatment of diabetes mellitus and hypertension.

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Section: Methodsmentioning

confidence: 99%

“…(S)-1-(4-(4-amino-4-(1H-benzo[d]imidazol-2-yl)butyl) guanidine (IVa) is obtained as a gray powder. For analytical purposes, the product (IVa) is additionally was purified by prep-HPLC (Phenomenex Luna C18 100 mm × 40 mm × 5 μm, 70 Histidine (155 mg, 1.0 mmol) and benzene-1,2-diamine (108 mg, 1.0 mmol), dissolve in 5 mL anhydrous glacial acetic acid (AGAA) in a 20 mL round bottom flask, place in a system with a reflux condenser and a Dean-Stark nozzle. Boil with the reflux condenser and extract 3 mL of AGAA.…”

Section: Materials and Equipmentmentioning

confidence: 99%

Molecular Modeling, Synthesis, and Antihyperglycemic Activity of the New Benzimidazole Derivatives – Imidazoline Receptor Agonists

Martynov,

Farber,

Bomko

et al. 2024

DDDT

View full text Add to dashboard Cite

show abstract

“…Advanced breast cancer can be successfully treated with Ixabepilone combined with Capecitabine [13][14][15][16]. For the method development and validation sections of current research work, referred the articles [17][18][19].…”

Section: Introductionmentioning

confidence: 99%

A validated stability‐indicating reversed‐phase liquid chromatography method for the quantification of Ixabepilone (Oncology drug) in the parenteral dosage form

Nekkalapudi

Srinivasu

Pippalla

et al. 2023

Separation Science Plus

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A quick and simple isocratic stability indicating method has been developed for the quantification of Ixabepilone in active pharmaceutical ingredient and injection dose formulation using reversed phase‐high‐performance liquid chromatography. Based on the response of Ixabepilone and impurities, the method was developed on a Symmetry C18 (150 × 4.6) mm, 5‐micron (Waters) column. An isocratic mobile phase consisted of pH 4.7 acetate buffer (10 mM) and acetonitrile in the composition of 60:40 v/v at 1.0 ml/min flow rate with a run time of 15 min, and Ixabepilone was eluted at about retention time of 5.1 min. The developed method is validated to meet International Conference on Harmonization standards. Linearity of Ixabepilone was established for the concentration range 0.050 to 0.15 mg/ml (r2 > 0.999) with respect to working concentration 0.10 mg/ml. Recovery was established from 50% (0.050 mg/ml) to 150% (0.15 mg/ml) of the target concertation (0.10 mg/ml). Precision and Intermediate precision met the acceptance criteria as per International Conference on Harmonization Q2(R1). It was proved that the stability indicating nature for quantifying Ixabepilone in Ixabepilone active pharmaceutical ingredient and drug product. As a result, the assay of Ixabepilone can be analyzed using this method for pharmaceutical development and quality control.

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Section: Introductionmentioning

confidence: 99%

“…In this exploration of work, method development and validation followed Pippalla, Jillelamudi, and Nekkalapudi (2022), Pippalla, Nekkalapudi, and Jillellamudi (2022), Nekkalapudi, Srinivasu, et al (2022), Nekkalapudi, Veldi, and Pippalla (2022), and Kasa et al (2012). In the quality‐control division of the pharmaceutical sector, the quantification of the active compounds and their all‐organic impurities in pharmaceutical products is necessary.…”

Section: Introductionmentioning

confidence: 99%

A stability‐indicating, reversed‐phase HPLC method for quantification of assay and organic impurities in doxycycline hyclate bulk and parenteral dosage forms

Pippalla

Nekkalapudi²,

Jillellamudi

et al. 2023

Biomedical Chromatography

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The aim of this study is to develop a stability‐indicating, reversed‐phase HPLC method for the quantification of assay and organic impurities (process and degradation) of doxycycline hyclate in a doxycycline injectable formulation. Both the active and dosage forms are officially present in the USP monograph, and assay and impurity methods are provided by separate UPLC techniques, which are highly sensitive to the flow rate and temperature, considering the quality control requirements and user‐friendliness. A simple stability‐indicating HPLC method with a shorter run time was developed for the simultaneous quantification of assay and impurity. The method was developed using HPLC with a gradient program and a reversed‐phase Waters XBridge BEH C8 column (150 × 4.6 mm, 3.5 μm i.d.). Mobile phase A consisted of phosphate buffer (pH 8.5, 25 mM potassium phosphate, 2 mM ethylenediaminetetraacetic acid, and 0.5 ml of triethylamine). Mobile phase B consisted of methanol with a flow rate of 1.7 ml/min, a column temperature of 55°C, a UV wavelength of 270 nm, and an injection volume of 25 μl. Modern research represents a concomitant method for quantifying assay and organic impurities of doxycycline hyclate (active form) and doxycycline for injection (dosage form). The assay and impurity method were validated per United States Pharmacopeia (USP) 1225 and International Conference on Harmonization (ICH) guidelines. The retention time of doxycycline and degradation impurity, 4‐epidoxycycline, was about 9.8 and 6.4 min, respectively. The linearity range of doxycycline and 4‐epidoxycycline was 0.5–150 and 0.5–18 μg/ml, respectively. The percentage of recovery of doxycycline and 4‐epidoxycycline was 98.7–100.6% and 88.0–112.0%. Validation of the analytical method demonstrated that the method is suitable, specific, linear, accurate, precise, rugged, and stability indicating for estimating the assay, known and degraded impurities of doxycycline, and doxycycline for injection.

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A Novel RP-HPLC Method for Estimating Fulvestrant, Benzoyl Alcohol, and Benzyl Benzoate in Injection Formulation

Cited by 11 publications

References 14 publications

Molecular Modeling, Synthesis, and Antihyperglycemic Activity of the New Benzimidazole Derivatives – Imidazoline Receptor Agonists

Molecular Modeling, Synthesis, and Antihyperglycemic Activity of the New Benzimidazole Derivatives – Imidazoline Receptor Agonists

A validated stability‐indicating reversed‐phase liquid chromatography method for the quantification of Ixabepilone (Oncology drug) in the parenteral dosage form

A stability‐indicating, reversed‐phase HPLC method for quantification of assay and organic impurities in doxycycline hyclate bulk and parenteral dosage forms

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