LC–MS/MS characterization of the forced degradation products of ezetemibe: Development and validation of a stability-indicating UPLC method

Prasad, KDV; Velpuri, Venkatappaiah; Alegete, Pallavi; Albaseer, Saeed S.; Mukkanti, K.; Das, Parthasaradhi

doi:10.1016/j.jtusci.2015.08.001

Cited by 9 publications

(7 citation statements)

References 9 publications

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“…Peak purity for the peaks acquired from various degradation tests was observed utilizing tools from the empower programme, and it was declared that the FEL peak was pure and homogenous from all examined stress samples. Mass balance values were determined from the stressed samples, and it was found that all of the results are greater than 99.6% (Table 3), which is consistent with the findings of earlier studies [24]. Thus, it was determined that the devised technique was stable and specific to Imp 1 and its degradation products.…”

Section: Dp1 (M/z: 356)supporting

confidence: 86%

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Sensitive and validated UPLC-MS/MS method for the identification and characterization of forced degradation products for felodipine

Babu

Kumar

Naresh³

et al. 2024

AChrom

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A rapid, stability indicating reverse phase liquid chromatographic method was developed for the determination of purity of Felodipine in active pharmaceutical substance form in the presence of its impurity and its degradation products. To develop the method which is also compatible to liquid chromatographic mass spectroscopic technique. The developed method is also used to determine the assay of Felodipine in bulk drug form. The drug is subjected to various stress conditions like acidic, basic, oxidation, UV light and thermal conditions. Considerable degradation was observed during base hydrolysis. Two degradation products were identified. The Waters Acquity UPLC BEH C18, 2.1 × 100 mm, 1.7 µm Column was used to achieve chromatographic separation. The gradient conditions, diluent and injection volume were optimized to achieve the acceptable resolution between impurities and its degradation products from Felodipine and to get good peak shapes. The masses were determined for main compound and its identified degradation products. Further, the characterization studies for main compound and its degradation products were performed using LCMSMS Q-TOF.

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Section: Dp1 (M/z: 356)supporting

confidence: 86%

“…The two molecular ions fragments formed under the base stress condition which are as follows: 1. [24].…”

Section: Dp1 (M/z: 356)mentioning

confidence: 99%

Sensitive and validated UPLC-MS/MS method for the identification and characterization of forced degradation products for felodipine

Babu

Kumar

Naresh³

et al. 2024

AChrom

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“…The chemical degradation assays on HO-AAVPA were followed using HPLC (Fig. 2 ) to separate the generate by-products to be analyzed (molecular weight) by LC–MS/MS as was for ezetemibe 39 . Once the HO-AAVPA was subjected to force degradation studies (acid and alkaline conditions, oxidation, heat, sunlight, the oxidation), only the sunlight generates a by-product that correspond to dimmer HO-AAVPA (Fig.…”

Section: Resultsmentioning

confidence: 99%

PAMAM-G4 protect the N-(2-hydroxyphenyl)-2-propylpentanamide (HO-AAVPA) and maintain its antiproliferative effects on MCF-7

Ortiz-Morales

García-Vázquez²,

Fragoso-Vázquez³

et al. 2023

Sci Rep

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Our work group designed and synthesized a promissory compound N-(2-hydroxyphenyl)-2-propylpentanamide (HO-AAVPA). The HO-AAVPA is a HDAC1 inhibitor and antiproliferative in cancer cell lines. However, HO-AAVPA is poor water solubility and enzymatically metabolized. In this work, the fourth-generation poly(amidoamine) dendrimer (PAMAM-G4) was used as a drug deliver carrier of HO-AAVPA. Moreover, HO-AAVPA and HO-AAVPA-PAMAM complex were submitted to forced degradation studies (heat, acid, base, oxidation and sunlight). Also, the HO-AAVPA-PAMAM-G4 complex was assayed as antiproliferative in a breast cancer cell line (MCF-7). The HO-AAVPA-PAMAM-G4 complex was obtained by docking and experimentally using three pH conditions: acid (pH = 3.0), neutral (pH = 7.0) and basic (pH = 9.0) showing that PAMAM-G4 captureand protect the HO-AAVPA from forced degradation, it is due to sunlight yielded a by-product from HO-AAVPA. In addition, the PAMAM-G4 favored the HO-AAVPA water solubility under basic and neutral pH conditions with significant difference (F(2,18) = 259.9, p < 0.001) between the slopes of the three conditions being the basic condition which solubilizes the greatest amount of HO-AAVPA. Finally, the HO-AAVPA-PAMAM-G4 complex showed better antiproliferative effects on MCF-7 (IC50 = 75.3 μM) than HO-AAVPA (IC50 = 192 μM). These results evidence that PAMAM-G4 complex improve the biological effects of HO-AAVPA.

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“…The same thing shows that the MCP was affected by acidic medium to a certain level. It is an indication for both bulk drug and generic product manufacturers to optimize the critical quality aspects to evade the exposure of HCl during the manufacturing pro- cess (Kancherla et al, 2016;Babu et al, 2018).…”

Section: Rp-hplc Methods Development For the Stabilityindicating Technmentioning

confidence: 99%

LC-MS characterization of acid degradation products of metoclopramide: Development and validation of a stability-indicating RP-HPLC method

Valavala¹,

Seelam²,

Subbaiah³

et al. 2020

ijrps

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The present study aims to develop a simple, accurate and specific stability-indicating RP-HPLC technique for the analysis of metoclopramide in the presence of its stress degradation products and characterization of degradation compounds by LC-MS/MS analysis. As per ICH Q1A-R2 guidelines, the drug was exposed to acid hydrolytic stress condition. Three degradation products were formed for MCP in acid hydrolysis. The liquid chromatography was processed on a Luna C18-(2) 100A,250×4.6mm 5micron column using an isocratic mobile phase consisting of 0.1% formic acid in water-acetonitrile (20:80, v/v) by adjusting the mobile phase at 1 ml/min flow rate with wavelength detection at 273 nm. The developed procedure was applied to LC-MS/MS (liquid chromatography-tandem mass spectrometry) for the characterization of all the degradant components. Total new three degradation compounds were recognized and identified by LC-MS/MS. The developed RP-HPLC technique was validated as per the ICH Q2-R1 guidelines. Limit of detection and limit of quantification values of MCP were evaluated from the linearity graph and were found to be 5.23 µg/ml and 17.44 µg/ml. Accuracy study was established at 80.0, 100.0 and 120.0 µg/ml concentration levels and the findings were found in the range of 98.4% - 101.8%. The linearity of the technique was assessed over the drug concentration range of 50.0 µg/ml to 250.0 µg/ml and the regression equation, slope and correlation coefficient values were found to be y = 10618x + 1623.2, 10618 and 0.9996 respectively. The developed technique was uninterruptedly applied for the quantification of metoclopramide inactive pharmaceuticals.

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LC–MS/MS characterization of the forced degradation products of ezetemibe: Development and validation of a stability-indicating UPLC method

Cited by 9 publications

References 9 publications

Sensitive and validated UPLC-MS/MS method for the identification and characterization of forced degradation products for felodipine

Sensitive and validated UPLC-MS/MS method for the identification and characterization of forced degradation products for felodipine

PAMAM-G4 protect the N-(2-hydroxyphenyl)-2-propylpentanamide (HO-AAVPA) and maintain its antiproliferative effects on MCF-7

LC-MS characterization of acid degradation products of metoclopramide: Development and validation of a stability-indicating RP-HPLC method

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