Validated Stability-Indicating HPLC and UPLC Assay Methods for the Determination of Entacapone in Pharmaceutical Dosage Forms

Gümüştaş, Mehmet; Uslu, Bengi; Aboul‐Enein, Hassan Y.

doi:10.1007/s10337-014-2758-x

Cited by 10 publications

(5 citation statements)

References 9 publications

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“…To solve these problems in liquid chromatography, previous investigators have increased the HPLC analysis time and/or applied more advanced instruments such as ultra‐high‐pressure liquid chromatography (UPLC) systems (Sun et al., ; Zhang et al., ). However, UPLC systems have some disadvantages compared with HPLC systems, such as higher instrument prices, column back‐pressure levels, and high maintenance costs (Gumustas, Kurbanoglu, Uslu, & Ozkan, ; Gumustas, Uslu, Ozkan, & Aboul‐Enein, ). Therefore, in this study, we used an HPLC system instead of a UPLC system.…”

Section: Discussionmentioning

confidence: 99%

pH‐adjusted solvent extraction and reversed‐phase HPLC quantification of isoflavones from soybean (Glycine max (L.) Merr.)

Cho¹,

Jung

Nam

et al. 2020

Journal of Food Science

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Soybeans, Glycine max (L.) Merr., are among the most important food crops worldwide. Isoflavones are major bioactive phytochemicals in soybeans, and have a variety of health benefits, including antioxidative, antiatherosclerotic, antiinflammatory, and weak estrogen‐like effects. The isoflavone content and composition of soybeans vary according to the cultivar and the extraction solvent conditions. Therefore, we investigated the effects of three different solvent pHs (1.0, 5.5, and 10.0) on the isoflavone, total phenolic, and total flavonoid contents and antioxidant capacities of eight soybean cultivars developed in Korea. Twelve isoflavones in soybeans were efficiently separated and identified on a reversed‐phase high‐performance liquid chromatography (HPLC) system. The percentage distribution of isoflavones measured by HPLC in the eight soybean cultivars at various extraction pHs decreased as follows: malonyl isoflavones (67.2% to 81.3%) > isoflavone glucosides (16.2% to 29.0%; as nonacylated form) > acetyl isoflavones (1.6% to 5.9%). The highest contents of isoflavone glucosides, malonyl derivatives, and acetyl derivatives were extracted at solvent pHs of 10.0, 1.0, and 5.5, respectively. The solvent extraction at pH 1.0 yielded a lower total isoflavone content than those at pHs 5.5 and 10.0. However, the highest total phenolic and flavonoid contents were extracted from soybeans at pH 1.0. Soybeans extracted at pH 10.0 displayed the highest antioxidant capacities in the 2,2′‐azino‐bis(3‐ethylbenzothiazoline‐6‐sulfonic acid) radical assay. Taken together, these results suggest that proper solvent pH adjustment is needed to maximize the extraction of targeted forms of isoflavones from soybeans. Practical Application Soybeans contain a variety of bioactive compounds, including isoflavones, which function as antioxidants and weak phytoestrogens. Chemical and instrumental analyses can facilitate the selection of soybean cultivars with high amounts of isoflavones for soybean breeding and isoflavone‐enriched product development. Proper solvent pH adjustment allows for the efficient extraction of high amounts of targeted isoflavone subgroups (acetyl and malonyl forms) from soybeans for functional food products.

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Section: Discussionmentioning

confidence: 99%

pH‐adjusted solvent extraction and reversed‐phase HPLC quantification of isoflavones from soybean (Glycine max (L.) Merr.)

Cho¹,

Jung

Nam

et al. 2020

Journal of Food Science

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“…The columns show superior performance, and the ultra-high pressure liquid chromatography pump offers precise gradient control, low diffusion, a low cross-contamination auto-sampler system, a high-speed detector, and comprehensive hardware and software. The peak capacity, analysis efficiency, and sensitivity are greatly improved compared with conventional HPLC, providing a good platform for the separation analysis of complex systems (Gumustas et al, 2014;Hedaya et al, 2017;Wu et al, 2017). Time-of-flight MS (TOF-MS) can provide accurate molecular mass (Zhang et al, 2018).…”

Section: Introductionmentioning

confidence: 99%

UPLC-Q-TOF-MS Study of the Mechanism of THSWD for Breast Cancer Treatment

et al. 2020

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Taohong Siwu decoction (THSWD) is a classic traditional Chinese medicine (TCM) prescription that is widely used in the clinical treatment of gynecological and cerebrovascular diseases. Here we used a method that coupled ultra-performance liquid chromatography to quadrupole time-of-flight mass spectrometry (UPLC-Q-TOF-MS) in which both positive and negative ion modes were established to investigate the major constituents in THSWD. A Waters ACQUITY UPLC BEH C18 column (2.1 mm×100 mm, 1.7 mm) was used to separate the aqueous extract of THSWD. The mobile phase consisted of 0.1% aqueous formic acid (A) and acetonitrile (B). Ninety-five components were identified in two different ion modes, including aromatic acids, flavones, polysaccharides, volatile oils monoterpene glycosides, aromatic cyanogenic glycosides, and others. Pathological changes in tumors and serum expression of interleukin-4 in a mouse model of breast cancer were detected after THSWD treatment. The results showed that THSWD had obvious therapeutic effects. This study establishes a material basis for the use of THSWD in the treatment of breast cancer.

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“…They are much lower than those obtained by all reported methods. 6,7,[9][10][11][12][13][14][15][16][17][18][19][20][21][22][23][24][25][26][27] Repeatability (intra-day assay), reproducibility (inter-day assay), precision and accuracy 56,57 of the described method (Table II) were evaluated by performing five replicate measurements for various concentrations of ENT over 1 day (intra-day assay) and for 3 days (interday assay). Satisfactory mean recoveries %R, relative standard deviations %RSD and relative error %RE were achieved indicating the repeatability, reproducibility, precision and accuracy of the described method.…”

Section: Daymentioning

confidence: 99%

“…However, due to its vital importance, several analytical methods were reported in the literature for its determination in formulations or in biological fluids. They included liquid chromatography (LC), 6 liquid chromatography-tandem mass spectrometry (LC-ESI-MS/MS), 9 high performance liquid chromatography (HPLC), 7,[10][11][12][13][14][15][16] ultra performance liquid chromatography (UPLC), 16,17 spectrophotometry 11,[18][19][20][21][22][23] and voltammetry. [24][25][26][27] The typical low limit of quantification (LOQ) of ENT plasma concentrations for healthy volunteers following administration of a single oral dose of 200 mg ENT were in the range of 10 ng mL −1 (3.28 × 10 −8 mol L −1 ) to 25 ng mL −1 (8.19 × 10 −8 mol L −1 ).…”

mentioning

confidence: 99%

“…[24][25][26][27] The typical low limit of quantification (LOQ) of ENT plasma concentrations for healthy volunteers following administration of a single oral dose of 200 mg ENT were in the range of 10 ng mL −1 (3.28 × 10 −8 mol L −1 ) to 25 ng mL −1 (8.19 × 10 −8 mol L −1 ). [5][6][7]9,13 Thus, the z E-mail: hseldesoky@hotmail.com published HPLC, [10][11][12][14][15][16] UPLC, 16,17 and spectrophotometric 11,[18][19][20][21][22][23] methods for the determination of ENT in formulations are not sensitive enough (LOQ = 1.77 × 10 −7 to 1.60 × 10 −5 mol L −1 ) to assay the drug in biological fluids. Although, the other chromatographic methods 6,7,9,13 are sensitive enough for assay of ENT in biological fluids, they are complicated, expensive and require sample pretreatment and time-consuming liquid-liquid or solid-phase extraction steps prior to the analysis or require high strength ionic buffered mobile phases 6,10,[12][13][14][15] (which are hazardous for column efficiency and need prolonged time for column saturation and washing).…”

mentioning

confidence: 99%

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Electrochemistry of the COMT Enzyme Inhibitor Entacapone and Its Determination in Pharmaceutical Formulation and Human Blood-Pharmacokinetic Study

Ghoneim

El‐Desoky

2015

J. Electrochem. Soc.

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Entacapone (ENT) is a potent inhibitor of catechol-O-methyltransferase enzyme. ENT is reduced via two irreversible cathodic waves over the pH range 2.0–11.5. It has strong interfacial adsorptive behavior onto Hg electrode surface. Langmuir isotherm indicated monolayer adsorption and the equilibrium parameter RL value (0.40 – 0.93) indicated that sorption process was favorable. A monolayer surface coverage of 6.06 × 10−10 mol cm−2 was estimated and each adsorbed ENT molecule occupied an area of 0.27 nm2. Taking advantage of the adsorption features of ENT, a sensitive and selective square-wave adsorptive cathodic stripping voltammetric (SW-AdCSV) method was developed for trace determination of ENT in pure form, commercial formulations (in Comtan tablets; as a single active drug and in Stalevo 200 tablets; as tertiary mixture of ENT, levodopa and carbidopa) and in human serum. Limits of quantification (LOQ) of 5.0 × 10−10 and 1.3 × 10−9 mol L−1 ENT were achieved in pure form and in spiked human serum, respectively. This analysis was carried out without addition of any surfactant, extraction of the drug and interference from some common excipients, co-formulated and co-administrated drugs. The proposed method has also been successfully applied for assay of ENT in real plasma samples and seems to be suitable for therapeutic drug monitoring purposes.

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Validated Stability-Indicating HPLC and UPLC Assay Methods for the Determination of Entacapone in Pharmaceutical Dosage Forms

Cited by 10 publications

References 9 publications

pH‐adjusted solvent extraction and reversed‐phase HPLC quantification of isoflavones from soybean (Glycine max (L.) Merr.)

pH‐adjusted solvent extraction and reversed‐phase HPLC quantification of isoflavones from soybean (Glycine max (L.) Merr.)

UPLC-Q-TOF-MS Study of the Mechanism of THSWD for Breast Cancer Treatment

Electrochemistry of the COMT Enzyme Inhibitor Entacapone and Its Determination in Pharmaceutical Formulation and Human Blood-Pharmacokinetic Study

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