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Development of Sample Preparation and Analytical Methods
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Development of Sample Preparation and Analytical Methods

A special issue of Molecules (ISSN 1420-3049). This special issue belongs to the section "Analytical Chemistry".

Deadline for manuscript submissions: closed (16 September 2023) | Viewed by 10762

Special Issue Editors

Prof. Dr. Philiswa Nosizo Nomngongo

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Guest Editor
Department of Chemical Sciences, University of Johannesburg, Doornfontein 2028, Gauteng, South Africa
Interests: nanotechnology; nanomaterials; chemometrics; sample preparation; environmental analytical chemistry
Special Issues, Collections and Topics in MDPI journals
Prof. Dr. Lawrence Mzukisi Madikizela

E-Mail Website
Guest Editor
Institute for Nanotechnology and Water Sustainability, University of South Africa, Johannesburg, South Africa
Interests: analytical chemistry; environmental monitoring; chromagraphy; molecularly imprinted polymer; pharmaceticals
Prof. Dr. Vusumzi E. Pakade

E-Mail Website
Guest Editor
Department of Chemistry, Faculty of Vaal University of Technology, Vanderbijlpark, South Africa
Interests: analytical chemistry; molecularly imprinted polymer; sample preparation; emerging contaminants; adsorbents

Special Issue Information

Dear Colleagues,

Inexorable industrialization aimed at improving the quality of life is unfortunately a threat to scarce natural resources like water. Numerous studies have detected a number of toxic organic and inorganic contaminants in environmental water bodies and attributed their occurrence to both domestic and industrial activities. Contaminants of emerging concern (CECs), pharmaceuticals and personal care products, and heavy metals have attracted widespread interest from researchers. Alarming concerns about environmental pollution have led to more research being focused on the development of methodologies for environmental analysis, monitoring and remediation. However, the fate and impact of emerging pollutants in the aquatic environment are not well-documented nor understood. Many researchers have reported the application of nanotechnology in environmental analytical chemistry owing to the advantage of utilizing a variety of nanomaterials with distinct properties and flexibility. Nanomaterials are used to profile the occurrence and distribution of pollutants in water systems, and to ascertain the contaminant concentration levels. Such materials lead to improved selectivity, adsorption, and extraction efficiency toward the target analytes, and enhance the sensitivity of the complete analytical method. In environmental analysis, the use of nanomaterials has received considerable attention because they can provide substantial simplification of the analytical procedures.

Prof. Dr. Philiswa Nosizo Nomngongo
Prof. Dr. Lawrence Mzukisi Madikizela
Prof. Dr. Vusumzi E. Pakade
Guest Editors

Manuscript Submission Information

Manuscripts should be submitted online at www.mdpi.com by registering and logging in to this website. Once you are registered, click here to go to the submission form. Manuscripts can be submitted until the deadline. All submissions that pass pre-check are peer-reviewed. Accepted papers will be published continuously in the journal (as soon as accepted) and will be listed together on the special issue website. Research articles, review articles as well as short communications are invited. For planned papers, a title and short abstract (about 100 words) can be sent to the Editorial Office for announcement on this website.

Submitted manuscripts should not have been published previously, nor be under consideration for publication elsewhere (except conference proceedings papers). All manuscripts are thoroughly refereed through a single-blind peer-review process. A guide for authors and other relevant information for submission of manuscripts is available on the Instructions for Authors page. Molecules is an international peer-reviewed open access semimonthly journal published by MDPI.

Please visit the Instructions for Authors page before submitting a manuscript. The Article Processing Charge (APC) for publication in this open access journal is 2700 CHF (Swiss Francs). Submitted papers should be well formatted and use good English. Authors may use MDPI's English editing service prior to publication or during author revisions.

Keywords

  • environmental analysis
  • molecularly imprinted polymers
  • solid extraction
  • sample preparation
  • organic pollutants
  • inorganic pollutants
  • food analysis
  • nanomaterials

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Published Papers (5 papers)

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Research

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16 pages, 2061 KiB  
Article
Analytical Quality by Design-Compliant Development of a Cyclodextrin-Modified Micellar ElectroKinetic Chromatography Method for the Determination of Trimecaine and Its Impurities
by Luca Marzullo, Roberto Gotti, Serena Orlandini, Patricie Slavíčková, Jakub Jireš, Michal Zapadlo, Michal Douša, Pavla Nekvapilová, Pavel Řezanka and Sandra Furlanetto
Molecules 2023, 28(12), 4747; https://doi.org/10.3390/molecules28124747 - 13 Jun 2023
Cited by 2 | Viewed by 1531
Abstract
In 2022, the International Council for Harmonisation released draft guidelines Q2(R2) and Q14, intending to specify the development and validation activities that should be carried out during the lifespan of an analytical technique addressed to assess the quality of medicinal products. In the [...] Read more.
In 2022, the International Council for Harmonisation released draft guidelines Q2(R2) and Q14, intending to specify the development and validation activities that should be carried out during the lifespan of an analytical technique addressed to assess the quality of medicinal products. In the present study, these recommendations were implemented in Capillary Electrophoresis method development for the quality control of a drug product containing trimecaine, by applying Analytical Quality by Design. According to the Analytical Target Profile, the procedure should be able to simultaneously quantify trimecaine and its four impurities, with specified analytical performances. The selected operative mode was Micellar ElectroKinetic Chromatography employing sodium dodecyl sulfate micelles supplemented with dimethyl-β-cyclodextrin, in a phosphate-borate buffer. The Knowledge Space was investigated through a screening matrix encompassing the composition of the background electrolyte and the instrumental settings. The Critical Method Attributes were identified as analysis time, efficiency, and critical resolution values. Response Surface Methodology and Monte Carlo Simulations allowed the definition of the Method Operable Design Region: 21–26 mM phosphate-borate buffer pH 9.50–9.77; 65.0 mM sodium dodecyl sulfate; 0.25–1.29% v/v n-butanol; 21–26 mM dimethyl-β-cyclodextrin; temperature, 22 °C; voltage, 23–29 kV. The method was validated and applied to ampoules drug products. Full article
(This article belongs to the Special Issue Development of Sample Preparation and Analytical Methods)
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11 pages, 2334 KiB  
Article
Response Surface Optimization of Dispersive Solid-Phase Extraction Combined with HPLC for the Rapid Analysis of Multiple Coccidiostats in Feed
by Haolan Tang, Shudan Liao, Jian Yang, Lilong Zhang, Aijuan Tan, Deyuan Ou, Shiming Lv and Xuqin Song
Molecules 2022, 27(23), 8559; https://doi.org/10.3390/molecules27238559 - 5 Dec 2022
Cited by 2 | Viewed by 1467
Abstract
Since antimicrobials were banned as feed additives, coccidiostats with favorable anticoccidial action and growth promotion have been widely used in the breeding industry. The monitoring of coccidiostats in feed is necessary, while the current methods based on mass-spectrometer analysis have limited applicability and [...] Read more.
Since antimicrobials were banned as feed additives, coccidiostats with favorable anticoccidial action and growth promotion have been widely used in the breeding industry. The monitoring of coccidiostats in feed is necessary, while the current methods based on mass-spectrometer analysis have limited applicability and matrix effects could interfere with the results. Accordingly, in the present paper, a rapid analytical strategy for the simultaneous determination of six synthetic coccidiostats in feed using high-performance liquid chromatography coupled with diode-array detection was developed. Coccidiostats in chicken feeds were extracted with the trichloroacetic acid–acetonitrile solution. The cleanup was performed by dispersive solid-phase extraction after the optimization of the response surface methodology. The method exhibited good linearity for target coccidiostats within the range of 0.05~20 µg/mL. Recoveries for six compounds in fortified feed samples were from 67.2% to 107.2% with relative standard deviations less than 9.6%. The limit of detection was 0.2~0.3 mg/kg. The successful application of the method in commercial feed verified that it is effective and sensitive for the rapid determination of multiple coccidiostats in chicken feeds. Full article
(This article belongs to the Special Issue Development of Sample Preparation and Analytical Methods)
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16 pages, 6147 KiB  
Article
A Simple Model to Estimate the Number of Metal Engineered Nanoparticles in Samples Using Inductively Coupled Plasma Optical Emission Spectrometry
by Nokwanda Hendricks, Olatunde Olatunji and Bhekumuzi Gumbi
Molecules 2022, 27(18), 5810; https://doi.org/10.3390/molecules27185810 - 8 Sep 2022
Cited by 2 | Viewed by 1822
Abstract
Accurate determination of the size and the number of nanoparticles plays an important role in many different environmental studies of nanomaterials, such as fate, toxicity, and occurrence in general. This work presents an accurate model that estimates the number of nanoparticles from the [...] Read more.
Accurate determination of the size and the number of nanoparticles plays an important role in many different environmental studies of nanomaterials, such as fate, toxicity, and occurrence in general. This work presents an accurate model that estimates the number of nanoparticles from the mass and molar concentration of gold nanoparticles (AuNPs) in water. Citrate-capped AuNPs were synthesized and characterized using transmission electron microscopy (TEM) and ultraviolet–visible spectroscopy (UV-vis). A mimic of environmental matrices was achieved by spiking sediments with AuNPs, extracted with leachate, and separated from the bulk matrix using centrifuge and phase transfer separation techniques. The quantification of AuNPs’ molar concentration on the extracted residues was achieved by inductively coupled plasma optical emission spectroscopy (ICP-OES). The molar concentrations, an average diameter of 27 nm, and the colloidal suspension volumes of AuNPs enable the calculation of the number of nanoparticles in separated residues. The plot of the number of AuNPs against the mass of AuNPs yielded a simple linear model that was used to estimate the number of nanoparticles in the sample using ICP-OES. According to the authors’ knowledge, this is the first adaptation of the gravimetric method to ICP-OES for estimating the number of nanoparticles after separation with phase transfer. Full article
(This article belongs to the Special Issue Development of Sample Preparation and Analytical Methods)
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Review

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15 pages, 5093 KiB  
Review
Current Sample Preparation Methods and Determination Techniques for the Determination of Phthalic Acid Ester Plasticizers in Edible Oils
by Menghui Qi, Yanyan Li, Zheng Zhu, Bin Du and Di Chen
Molecules 2023, 28(13), 5106; https://doi.org/10.3390/molecules28135106 - 29 Jun 2023
Cited by 4 | Viewed by 2012
Abstract
In the process of production, processing, transportation, and storage of edible oils, the oils inevitably come into contact with plastic products. As a result, plasticizers migrate into edible oils, are harmful to human health, and can exhibit reproductive toxicity. Therefore, the determination of [...] Read more.
In the process of production, processing, transportation, and storage of edible oils, the oils inevitably come into contact with plastic products. As a result, plasticizers migrate into edible oils, are harmful to human health, and can exhibit reproductive toxicity. Therefore, the determination of plasticizers in edible oils is very important, and a series of sample preparation methods and determination techniques have been developed for the determination of plasticizers in edible oils. Phthalic acid ester (PAE) plasticizers are the most widely used among all plasticizers. This review aims to provide a comprehensive overview of the sample preparation methods and detection techniques reported for the determination of PAEs in edible oils since 2010, focusing on sample preparation methods of edible oils combined with various separation-based analytical techniques, such as gas chromatography (GC) and liquid chromatography (LC) with different detectors. Furthermore, the advantages, disadvantages, and limitations of these techniques as well as the prospective future developments are also discussed. Full article
(This article belongs to the Special Issue Development of Sample Preparation and Analytical Methods)
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20 pages, 4130 KiB  
Review
Advances on Hormones in Cosmetics: Illegal Addition Status, Sample Preparation, and Detection Technology
by Mengyue Li, Li Wang, Min Wang, Hua Zhao and Fengnian Zhao
Molecules 2023, 28(4), 1980; https://doi.org/10.3390/molecules28041980 - 20 Feb 2023
Cited by 3 | Viewed by 3020
Abstract
Owing to the rapid development of the cosmetic industry, cosmetic safety has become the focus of consumers’ attention. However, in order to achieve the desired effects in the short term, the illegal addition of hormones in cosmetics has emerged frequently, which could induce [...] Read more.
Owing to the rapid development of the cosmetic industry, cosmetic safety has become the focus of consumers’ attention. However, in order to achieve the desired effects in the short term, the illegal addition of hormones in cosmetics has emerged frequently, which could induce skin problems and even skin cancer after long-term use. Therefore, it is of great significance to master the illegal addition in cosmetics and effectively detect the hormones that may exist in cosmetics. In this review, we analyze the illegally added hormone types, detection values, and cosmetic types, as well as discuss the hormone risks in cosmetics for human beings, according to the data in unqualified cosmetics in China from 2017 to 2022. Results showed that although the frequency of adding hormones in cosmetics has declined, hormones are still the main prohibited substances in illegal cosmetics, especially facial masks. Because of the complex composition and the low concentration of hormones in cosmetics, it is necessary to combine efficient sample preparation technology with instrumental analysis. In order to give the readers a comprehensive overview of hormone analytical technologies in cosmetics, we summarize the advanced sample preparation techniques and commonly used detection techniques of hormones in cosmetics in the last decade (2012–2022). We found that ultrasound-assisted extraction, solid phase extraction, and microextraction coupled with chromatographic analysis are still the most widely used analytical technologies for hormones in cosmetics. Through the investigation of market status, the summary of sample pretreatment and detection technologies, as well as the discussion of their development trends in the future, our purpose is to provide a reference for the supervision of illegal hormone residues in cosmetics. Full article
(This article belongs to the Special Issue Development of Sample Preparation and Analytical Methods)
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