Showing posts with label chromatography. Show all posts
Showing posts with label chromatography. Show all posts

Monday, 10 March 2025

Refining UPLC Methodology for Comprehensive Analysis of Molindone and Its Impurities | Chapter 6 | Recent Developments in Chemistry and Biochemistry Research Vol. 9

Background: Sensitive determination of molindone and its impurities to be developed for the molindone drug substance/products.

Aim: Effective chromatographic separation was achieved on a phenyl-hexyl stationary phase for the determination of molindone and its related impurities.

Methods: The economical and straightforward mobile phase combination delivered in gradient mode at a flow rate of 0.6 mL/min at 254 nm using the phenyl-hexyl column with the dimension of (50 × 2.1 mm, 1.9 µ particles) with the help of an ultra-performance liquid chromatography (UPLC) system.

Results: In the developed method, the resolution between molindone and its related compounds was more significant than 2.0. Regression analysis shows an r2 value (correlation coefficient square) greater than 0.999 for molindone and its associated compounds. This method could detect related compounds of molindone at a level below 0.009% with respect to a test concentration of 500 µg/mL for a 2.0 µL injection volume.

Conclusion: The method has shown good, consistent recoveries for related compounds (90-110%). The test solution was found to be stable in the diluent for 48 hours. The drug was subjected to stress conditions. The mass balance was found to be close to 99.3%. The validated method may be used for the routine analysis of the determination of related compounds of molindone from the bulk drug, pharmaceutical preparation, and other quality control samples of product development.

 

Author (s) Details

 

Balaji Nagarajan
Apicore LLC, East Windsor, New Jersey, 08520, United States.

 

Gunasekar Manoharan
New Jersey Bioscience Centre, 675 US Highway 1, North Brunswick, New Jersey, 08902, United States.

 

Ganapathy Narayanan Shanmugam
New Jersey Bioscience Centre, 675 US Highway 1, North Brunswick, New Jersey, 08902, United States.

 

Nataraj Palaniyappan
Shri Jagdishprasad Jhabarmal Tibrewala University, Rajasthan, 333001, India.

 

Abhinav Yarragunta
Majoring in Computer Engineering, Florida Semiconductor Institute, University of Florida, United States.

 

Please see the book here:- https://doi.org/10.9734/bpi/rdcbr/v9/3425

Friday, 7 March 2025

Rapid and Precise HPLC Analysis of Polymer Monomers in Bacillus sp. CYR1-Derived Polyhydroxyalkanoates Using Alkali Decomposition Pretreatment | Chapter 6 | Chemical and Materials Sciences: Research Findings Vol. 1

Background: Plastics are widely used worldwide due to their characteristics of being inexpensive, capable of mass production, lightweight, and highly durable. Although plastic, with its excellent properties, has become an essential part of daily life, it poses a significant threat because it does not decompose naturally in the environment and can persist for decades due to its stable physical properties. This has raised concerns about their impact on various ecosystems, including terrestrial and marine environments. Polyhydroxyalkanoates (PHA), produced by various bacteria and archaea, are biodegradable plastics with similar thermoplastic and elastic properties to conventional plastics.

Aim: The aim of the study is to develop a simple PHA quantification method using high-performance liquid chromatography (HPLC) with alkaline hydrolysis pretreatment.

Methods: Analysis was conducted using an HPLC (SHIMADZU, Kyoto, Japan) equipped with a UV-VIS detector (SHIMADZU, SPD-10AV) and a separation column (SHIMADZU, SCR model). The PHBV produced by Bacillus sp. CYR1 strain was quantified using both the developed method and GC analysis, and the quantification results were compared. A de-gassed peracetic acid solution (860 µL/L) was used as the mobile phase at a flow rate of 1.5 mL/min.

Results: By developing a simple PHA quantification method using alkaline hydrolysis pretreatment combined with HPLC, we attempted to quantify PHAs consisting of molecular chains longer than PHB by applying a simplified pretreatment process with HPLC. The retention times for standard reagents 2BE, 2PE, and 3HB were 11.1 minutes, 15.1 minutes, and 6.4 minutes, respectively. Additionally, the formation of 2BE and 2PE was observed from the PHA subjected to alkaline hydrolysis pretreatment, and the generated calibration curves demonstrated linearity.

As P(3HB-co-3HV) is a copolymer of 3-hydroxybutyrate (3HB) and 3-hydroxyvalerate (3HV), 2BE and 2PE are produced by the alkaline decomposition of P(3HB-co-3HV). For this, we used the equation P(3HB) = α × 2BE and P(3HV) = β × 2PE, because the production ratio α of 2BE from P(3HB) and the production ratio β of 2PE from P(3HV) are constant in the reaction under the same decomposition conditions.

The bacteria Chromobacterium violaceum and Bacillus sp. CYR1 were used to produce P(3HV) and P(3HB-co-3HV), respectively. The bacterium Bacillus sp. CYR1 produced 415 mg/L of P(3HB-co-3HV) when incubated with acetic acid and valeric acid as the carbon sources, whereas the bacterium C. violaceum produced 0.198 g of P(3HV)/g dry biomass when incubated with sodium valerate as the carbon source.

Since there is no standard sample for P(3HV), it was produced in this study from C. violaceum. From the ratio of the slopes of the calibration curve, the production ratios were determined as α =3.26 and β =3.30. These results indicate that short-chain-length PHA (scl-PHA) can be quantified easily and with high sensitivity by measuring the 2BE and 2PE contents of actual samples using the method proposed here.

Conclusion: It was confirmed that PHBV can be accurately quantified using the quantification method developed in this study. In the future, to assess the accuracy of the quantification results of PHBV in dried cell biomass, it will be necessary to validate the quantification method by performing GC analysis for comparison.

 

Author (s) Details

Young-Cheol Chang
Course of Chemical and Biological Engineering, Division of Sustainable and Environmental Engineering, Muroran Institute of Technology, Hokkaido 050-8585, Japan.

 

Please see the book here:- https://doi.org/10.9734/bpi/cmsrf/v1/4617

Thursday, 16 September 2021

Phytochemical Studies and Antioxidant Activity of Mauritia flexuosa and Mauritiella armata | Chapter 3 | New Visions in Biological Science Vol. 2

 Mauritia flexuosa and Mauritiella armata are Arecaceae plants that are common in Brazil. The phytochemical profile of the secretion commonly known as wine, produced from M. flexuosa, was investigated in this study. The antioxidant activity of hydroethanolic extracts of the two species' leaves, roots, and petioles, as well as flavonoids quantity and chromatographic profile, were determined using high performance liquid chromatography. High-performance liquid chromatography was used to determine the chromatographic profile, and spectrophotometry was used to quantify flavonoids and antioxidant activity. The presence of flavonoids and antioxidant activity was found in the extracts of all investigated structures from both species (M. flexuosa and M. armata). The presence of secondary metabolites found in other M. flexuosa structures was confirmed by the wine's phytochemical profile. The examined extracts have between three and nine chemicals, according to the chromatographic analyses. More research is needed to discover the active chemicals in both species.


Author (S) Details

Vanessa de Andrade Royo
Laboratory of Natural Products, State University of Montes Claros, Montes Claros/MG, Brazil.

Juliana Almeida Rocha
Laboratory of Natural Products, State University of Montes Claros, Montes Claros/MG, Brazil.

Kamylla Teixeira Santos
Laboratory of Natural Products, State University of Montes Claros, Montes Claros/MG, Brazil.

Jeane Ferreira Leal Freitas
Laboratory of Natural Products, State University of Montes Claros, Montes Claros/MG, Brazil.

Clarice Avelar Almeida
Laboratory of Natural Products, State University of Montes Claros, Montes Claros/MG, Brazil.

Elytania Veiga Menezes
Laboratory of Natural Products, State University of Montes Claros, Montes Claros/MG, Brazil.

Dario Alves de Oliveira
Laboratory of Natural Products, State University of Montes Claros, Montes Claros/MG, Brazil.

Murilo Malveira Brandão
Laboratory of Natural Products, State University of Montes Claros, Montes Claros/MG, Brazil.

Afranio Farias de Melo Júnior
Laboratory of Natural Products, State University of Montes Claros, Montes Claros/MG, Brazil.

View Book :- https://stm.bookpi.org/NVBS-V2/article/view/3709

Monday, 28 December 2020

Assessment of Lipid Composition in Medicinal Plants: Portulaca oleracea and Ficus thonningi | Chapter 7 | Recent Research Advances in Biology Vol. 3

 Medicinal features have been related for thousands of years to many species. The extracts of plants are commonly marketed as dietary supplements or tonics and advertised as health-beneficial. In order to evaluate the biochemical evidence for their therapeutic use as medicinal plants used in Nigeria, the lipid composition of these plants, Portulaca oleracea and Ficus thonningi, were analysed after extraction. P. oleracea lipids and F. Thonningi were extracted using chloroform and methanol (2:1), purified using Folch wash, and analysed to distinguish neutral and polar lipids and the different lipid groups using thin layer chromatography (TLC) and column chromatography. The percentage composition of the different fractions of lipids was determined. The TLC outcome showed some neutral lipids, linoleic acid (66.7%) and triolene (26.7%) in P. oleracea and triolene (70%) in F. Linolenic acid (50 percent), oleic acid (35 percent), phospholipids (5 percent) and diacylglycerol in P. olerecea thus in F. Thonnningi and polar lipids: They were triolene (70%), triglycerol (30%), phosphatidate (26.7%), phospholipid (13.3%), diacylglycerol (30%) (10 percent ). P. oleracea's overall lipid is 35 percent, and F. Thonningi stands at 30 percent. The biochemical evidence for the therapeutic use of purslane as a medicinal plant contains omega-3 fatty acids (50 percent) as well as omega-6 fatty acids (66.7 percent). The use of P. oleracea and F is encouraged by this work. As medicinal plants to combat the occurrence of CHD and to treat patients with risk factors for CHD, and to improve overall body health due to their ability to lower cholesterol levels, lower blood pressure is also due to their therapeutic and pharmacological properties.


Author(s) Details

Ochulayi P. Ora
Department of Biochemistry, National Research Institute for Chemical Technology, Zaria, Nigeria.

G. E. Anekwe

Department of Biochemistry, University of Jos, Plateau State, Nigeria.

View Book :- https://bp.bookpi.org/index.php/bpi/catalog/book/343