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Development of Analytical Methods in Food, Biological and Environmental Samples Determination II

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

Deadline for manuscript submissions: closed (31 August 2023) | Viewed by 25657

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Dr. Beata Polak

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Department of Physical Chemistry, Medical University of Lublin, Chodźki 4a, 20-093 Lublin, Poland
Interests: separation of biologically active compounds with chromatographic and electromigrational techniques; with the use of various mobile phases; including those containing surfactants
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Prof. Dr. Irina B. Karadjova

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Faculty of Chemistry and Pharmacy, University of Sofia Saint Kliment Ohridski, 1164 Sofia, Bulgaria
Interests: analytical atomic spectroscopy; speciation analysis; methods for separation and concentration; analysis of environmental samples, biological samples, food samples and beverages; development of analytical procedures; ecolegislation
Special Issues, Collections and Topics in MDPI journals

Dr. Anna Klimek Turek

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Department of Physical Chemistry, Medical University of Lublin, Chodźki 4a, 20-093 Lublin, Poland
Interests: liquid chromatography; high-performance liquid chromatography; chromatography

Special Issue Information

Dear Colleagues,

Scientists are still looking for novel and improved methods for the determination of many compounds in various sample types. The determined solutes have various origins and their actions toward humans or animals can be positive or negative. Thus, the development of a method that leads to the identification and then determination of minor or even ultra-minor compounds is important. The problem requiring a solution is not only the detection of a very small amount of analyte, but also how to deal with the matrix problem; the latter may be food, biological, or even environmental.

The successful separation and identification of compounds contribute to the achievement of many analytical methods. Distinguishing mixture compounds is based on differences in their physicochemical properties, involving various techniques (chromatographic, spectroscopic, electroanalytical, etc.), some of which enhance the sensitivity and are linked to various detection techniques (electrochemical, DAD, NMR, MS, etc.).

I encourage our colleagues to share their scientific achievements in the field of analytical method development in this Special Issue. Papers concerning the determination of solutes in food, biological, and environmental samples are especially welcome, but the Special Issue is not confined to these topics only.

Dr. Beata Polak
Dr. Irina B. Karadjova
Dr. Anna Klimek Turek
Guest Editors

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Keywords

determination of various compounds
electromigrational
chromatographic
spectral methods
various matrices

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Related Special Issues

Development of Analytical Methods in Food, Biological and Environmental Samples Determination in Molecules (10 articles)
Development of Analytical Methods in Food, Biological and Environmental Samples Determination: 3rd Edition in Molecules (2 articles)

Published Papers (11 papers)

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Research

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15 pages, 1620 KiB

Open AccessArticle

Monitoring Pharmaceuticals and Personal Care Products in Drinking Water Samples by the LC-MS/MS Method to Estimate Their Potential Health Risk

by Lucia Molnarova, Tatana Halesova, Marta Vaclavikova and Zuzana Bosakova

Molecules 2023, 28(15), 5899; https://doi.org/10.3390/molecules28155899 - 5 Aug 2023

Cited by 5 | Viewed by 2233

Abstract

(1) The occurrence and accumulation of pharmaceuticals and personal care products in the environment are recognized scientific concerns. Many of these compounds are disposed of in an unchanged or metabolized form through sewage systems and wastewater treatment plants (WWTP). WWTP processes do not completely eliminate all active substances or their metabolites. Therefore, they systematically leach into the water system and are increasingly contaminating ground, surface, and drinking water, representing a health risk largely ignored by legislative bodies. Especially during the COVID-19 pandemic, a significantly larger amount of medicines and protective products were consumed. It is therefore likely that contamination of water sources has increased, and in the case of groundwater with a delayed effect. As a result, it is necessary to develop an accurate, rapid, and easily available method applicable to routine screening analyses of potable water to monitor and estimate their potential health risk. (2) A multi-residue UHPLC-MS/MS analytical method designed for the identification of 52 pharmaceutical products was developed and used to monitor their presence in drinking water. (3) The optimized method achieved good validation parameters, with recovery of 70–120% of most analytes and repeatability achieving results within 20%. In real samples of drinking water, at least one analyte above the limit of determination was detected in each of the 15 tap water and groundwater samples analyzed. (4) These findings highlight the need for legislation to address pharmaceutical contamination in the environment. Full article

(This article belongs to the Special Issue Development of Analytical Methods in Food, Biological and Environmental Samples Determination II)

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13 pages, 3618 KiB

Open AccessArticle

An ESIPT-Based Fluorescent Probe for Aqueous Cu⁺ Detection through Strip, Nanofiber and Living Cells

by Zhao Cheng, Xilang Jin, Yinggang Liu, Lei Zheng and Hao He

Molecules 2023, 28(9), 3725; https://doi.org/10.3390/molecules28093725 - 26 Apr 2023

Cited by 7 | Viewed by 1619

Abstract

Constructed on the benzothiazole-oxanthracene structure, a fluorescent probe RBg for Cu⁺ was designed under the ESIPT mechanism and synthesized by incorporating amide bonds as the connecting group and glyoxal as the identifying group. Optical properties revealed a good sensitivity and a good linear relationship of the probe RBg with Cu⁺ in the concentration range of [Cu⁺] = 0–5.0 μmol L⁻¹. Ion competition and fluorescence-pH/time stability experiments offered further possibilities for dynamic Cu⁺ detection in an aqueous environment. HRMS analysis revealed a possible 1:1 combination of RBg and Cu⁺. In addition, colorimetric Cu⁺ detection and lysosome-targeted properties of the probe RBg were analyzed through RBg-doped PVDF nanofiber/test strips and RBg-Mito/Lyso trackers that were co-stained in living HeLa cells, enabling the probe’s future applications as real-time detection methods for dynamic Cu⁺ tracking in the lysosomes and Cu⁺ detection under diversified conditions. Full article

(This article belongs to the Special Issue Development of Analytical Methods in Food, Biological and Environmental Samples Determination II)

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14 pages, 3006 KiB

Open AccessArticle

Quantification of Ergot Alkaloids via Lysergic Acid Hydrazide—Development and Comparison of a Sum Parameter Screening Method

by Maximilian Kuner, Jan Lisec, Tatjana Mauch, Jörg Konetzki, Hajo Haase and Matthias Koch

Molecules 2023, 28(9), 3701; https://doi.org/10.3390/molecules28093701 - 25 Apr 2023

Cited by 1 | Viewed by 2183

Abstract

Ergot alkaloids are a group of mycotoxins occurring in products derived from various grasses (e.g., rye) and have been regulated in the EU recently. The new maximum levels refer to the sum of the six most common ergot alkaloids in their two stereoisomeric forms in different food matrices. Typically, these twelve compounds are individually quantified via HPLC-MS/MS or -FLD and subsequently summed up to evaluate food safety in a time-consuming process. Since all these structures share the same ergoline backbone, we developed a novel sum parameter method (SPM) targeting all ergot alkaloids simultaneously via lysergic acid hydrazide. After extraction and clean-up, in analogy to the current European standard method EN 17425 (ESM) for ergot alkaloid quantitation, the samples were derivatized by an optimized hydrazinolysis protocol, which allowed quantitative conversion after 20 min at 100 °C. The new SPM was evaluated against another established HPLC-FLD-based method (LFGB) and the HPLC-MS/MS-based ESM using six naturally contaminated rye and wheat matrix reference materials. While the SPM provided comparable values to the ESM, LFGB showed deviating results. Determined recovery rates, limits of detection and quantification of all three employed methods confirm that the new SPM is a promising alternative to the classical approaches for ergot alkaloid screening in food. Full article

(This article belongs to the Special Issue Development of Analytical Methods in Food, Biological and Environmental Samples Determination II)

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13 pages, 1194 KiB

Open AccessArticle

Validation of a Novel RP-HPLC Technique for Simultaneous Estimation of Lignocaine Hydrochloride and Tibezonium Iodide: Greenness Estimation Using AGREE Penalties

by Sana Hanif, Muhammad Ali Syed, Ahmad Junaid Rashid, Tareq Nafea Alharby, Mohammad M. Algahtani, Muteb Alanazi, Jowaher Alanazi and Rai Muhammad Sarfraz

Molecules 2023, 28(8), 3418; https://doi.org/10.3390/molecules28083418 - 13 Apr 2023

Cited by 1 | Viewed by 1896

Abstract

Herein, we reported an HPLC method for the simultaneous determination of tibezonium iodide (TBN) and lignocaine hydrochloride (LGN). The method was developed according to the International Conference for Harmonization guidelines (ICH) Q2R1 using Agilent^® 1260 with a mobile phase consisting of acetonitrile and phosphate buffer (pH 4.5) in a volumetric ratio of 70:30 and flowing through a C₈ Agilent^® column at 1 mL/min. The results revealed that TBN and LGN peaks were isolated at 4.20 and 2.33 min, respectively, with a resolution of 2.59. The accuracy of TBN and LGN was calculated to be 100.01 ± 1.72% and 99.05 ± 0.65% at 100% concentration, respectively. Similarly, the respective precision was 100.03 ± 1.61% and 99.05 ± 0.48%. The repeatability for TBN and LGN was found to be 99.05 ± 0.48% and 99.19 ± 1.72%, respectively, indicating that the method was precise. The respective regression co-efficient (r²) for TBN and LGN was found to be 0.9995 and 0.9992. Moreover, the LOD and LOQ values for TBN were 0.012 and 0.037 µg/mL, respectively, while for LGN, they were 0.115 and 0.384 µg/mL, respectively. The calculated greenness of the method for ecological safety was found to be 0.83, depicting a green contour on the AGREE scale. No interfering peaks were found when the analyte was estimated in dosage form and in volunteers’ saliva, depicting the specificity of the method. Conclusively, a robust, fast, accurate, precise and specific method was successfully validated to estimate TBN and LGN. Full article

(This article belongs to the Special Issue Development of Analytical Methods in Food, Biological and Environmental Samples Determination II)

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12 pages, 1738 KiB

Open AccessArticle

“Green” Extraction and On-Site Rapid Detection of Aflatoxin B1, Zearalenone and Deoxynivalenol in Corn, Rice and Peanut

by Zijing Li, Zepeng Li, Xintong Li, Qi Fan, Yinuo Chen and Guoqing Shi

Molecules 2023, 28(7), 3260; https://doi.org/10.3390/molecules28073260 - 6 Apr 2023

Cited by 2 | Viewed by 2356

Abstract

The common mycotoxins in polluted grains are aflatoxin B1(AFB1), zearalenone (ZEN) and deoxynivalenol (DON). Because of the potential threat to humans and animals, it is necessary to detect mycotoxin contaminants rapidly. At present, later flow immunoassay (LFIA) is one of the most frequently used methods for rapid analysis. However, multistep sample pretreatment processes and organic solvents are also required to extract mycotoxins from grains. In this study, we developed a one-step and “green” sample pretreatment method without using organic solvents. By combining with LFIA test strips and a handheld detection device, an on-site method for the rapid detection of AFB1, ZEN and DON was developed. The LODs for AFB1, ZEN and DON in corn are 0.90 μg/kg, 7.11 μg/kg and 10.6 μg/kg, respectively, and the working ranges are from 1.25 μg/kg to 40 μg/kg, 20 μg/kg to 2000 μg/kg and 35 μg/kg to 1500 μg/kg, respectively. This method has been successfully applied to the detection of AFB1, ZEN and DON in corn, rice and peanut, with recoveries of 89 ± 3%–106 ± 3%, 86 ± 2%–108 ± 7% and 90 ± 2%–106 ± 10%, respectively. The detection results for the AFB1, ZEN and DON residues in certified reference materials by this method were in good agreement with their certificate values. Full article

(This article belongs to the Special Issue Development of Analytical Methods in Food, Biological and Environmental Samples Determination II)

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16 pages, 4172 KiB

Open AccessArticle

Comparison of the Determination of Some Antihypertensive Drugs in Clinical Human Plasma Samples by Solvent Front Position Extraction and Precipitation Modes

by Kamila Jaglińska, Beata Polak, Anna Klimek-Turek, Emilia Fornal, Anna Stachniuk, Alicja Trzpil, Robert Błaszczyk and Andrzej Wysokiński

Molecules 2023, 28(5), 2213; https://doi.org/10.3390/molecules28052213 - 27 Feb 2023

Cited by 1 | Viewed by 1662

Abstract

The determination of the selected antihypertensive drugs in human plasma samples with the novel solvent front position extraction (SFPE) technique is presented. The SFPE procedure combined with LC-MS/MS analysis was used for the first time to prepare a clinical sample containing the drugs mentioned above from different therapeutic groups. The effectiveness of our approach was compared with the precipitation method. The latter technique is usually used to prepare biological samples in routine laboratories. During the experiments, the substances of interest and the internal standard were separated from other matrix components using a prototype horizontal chamber for thin-layer chromatography/high-performance thin-layer chromatography (TLC/HPTLC) with a moving pipette powered by a 3D mechanism, which distributed the solvent on the adsorbent layer. Detection of the six antihypertensive drugs was performed by liquid chromatography coupled to tandem mass spectrometry (LC–MS/MS) in multiple reaction monitoring (MRM) mode. Results obtained by SFPE were very satisfactory (linearity R² ≥ 0.981; %RSD ≤ 6%; LOD and LOQ were in the range of 0.06–9.78 ng/mL and 0.17–29.64 ng/mL, respectively). The recovery was in the range of 79.88–120.36%. Intra-day and inter-day precision had a percentage coefficient of variation (CV) in the range of 1.10–9.74%. The procedure is simple and highly effective. It includes the automation of TLC chromatogram development, which significantly reduced the number of manual operations performed, the time of sample preparation and solvent consumption. Full article

(This article belongs to the Special Issue Development of Analytical Methods in Food, Biological and Environmental Samples Determination II)

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21 pages, 2310 KiB

Open AccessArticle

The New Insight into the Effects of Different Fixing Technology on Flavor and Bioactivities of Orange Dark Tea

by Yuanfang Jiao, Yulin Song, Zhi Yan, Zhuanrong Wu, Zhi Yu, De Zhang, Dejiang Ni and Yuqiong Chen

Molecules 2023, 28(3), 1079; https://doi.org/10.3390/molecules28031079 - 20 Jan 2023

Cited by 5 | Viewed by 2365

Abstract

Peach leaf orange dark tea (ODT) is a fruity tea made by removing the pulp from peach leaf orange and placing dry Qingzhuan tea into the husk, followed by fixing them together and drying. Since the quality of traditional outdoor sunlight fixing (SL) is affected by weather instability, this study explored the feasibility of two new fixing methods, including hot air fixing (HA) and steam fixing (ST). Results showed that fixing method had a great impact on ODT shape, aroma, and taste. Compared with SL and ST, HA endowed ODT with higher fruit aroma, mellow taste, better coordination, and higher sensory evaluation score. Physical–chemical composition analysis showed that SL-fixed orange peel was higher than HA- or ST-fixed peel in the content of polyphenols, flavonoids, soluble protein, hesperidin and limonin, while HA has a higher content of volatile substances and contains more alcohols, aldehydes and ketones, and acid and esters than ST and SL. Activity analysis showed that HA was superior to ST or SL in comprehensive antioxidant activity and inhibitory activity against α-glucosidase. Comprehensive results demonstrated that HA has better performance in improving ODT quality and can replace the traditional SL method in production. Full article

(This article belongs to the Special Issue Development of Analytical Methods in Food, Biological and Environmental Samples Determination II)

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14 pages, 43588 KiB

Open AccessArticle

Structure and Flocculation of Ion Associates of Carrageenan and Poly(diallyldimethylammonium chloride) Depending on the Component Ratio

by Dorota Ziółkowska, Jan Lamkiewicz and Alexander Shyichuk

Molecules 2022, 27(22), 8075; https://doi.org/10.3390/molecules27228075 - 21 Nov 2022

Cited by 8 | Viewed by 1942

Abstract

Carrageenan is a polysaccharide of a plant origin, commonly used as a thickening and gelling agent in the food, pharmaceutical, and cosmetic industries. Due to the negative charges of its sulfate groups, carrageenan macromolecules strongly interact with oppositely charged polyions. The ionic complexes of carrageenan with poly(diallyldimethylammonium chloride) were obtained at the molar ratios 4:1, 2;1, 1:1, 1:2, and 1:4. The structure and characteristics of the polyanion-polycation associates were studied by XRD, IR, optical microscopy, and via sedimentation and particle size measurements. It was found that the suspended particles flocculate and settle fastest when the molar ratio of the polyions is near 1:1. Turbidimetric titration experiments enabled us to measure the molar ratio of cationic to anionic groups at the onset of flocculation, and the value in question was found to be 1:1.32. In other words, a mass of 511 mg carrageenan corresponds to one millimole of ester sulfate (monobasic) groups. The measurement of the onset of flocculation has been employed for the accurate determination of carrageenan in real samples of food products. The color and turbidity of the sample do not interfere with the determination results. Full article

(This article belongs to the Special Issue Development of Analytical Methods in Food, Biological and Environmental Samples Determination II)

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42 pages, 2268 KiB

Open AccessReview

Polymeric Materials in Speciation Analysis Based on Solid-Phase Extraction

by Ivanka Dakova, Tanya Yordanova and Irina Karadjova

Molecules 2024, 29(1), 187; https://doi.org/10.3390/molecules29010187 - 28 Dec 2023

Viewed by 1491

Abstract

Speciation analysis is a relevant topic since the (eco)toxicity, bioavailability, bio (geo)chemical cycles, and mobility of a given element depend on its chemical forms (oxidation state, organic ligands, etc.). The reliability of analytical results for chemical species of elements depends mostly on the maintaining of their stability during the sample pretreatment step and on the selectivity of further separation step. Solid-phase extraction (SPE) is a matter of choice as the most suitable and widely used procedure for both enrichment of chemical species of elements and their separation. The features of sorbent material are of great importance to ensure extraction efficiency from one side and selectivity from the other side of the SPE procedure. This review presents an update on the application of polymeric materials in solid-phase extraction used in nonchromatographic methods for speciation analysis. Full article

(This article belongs to the Special Issue Development of Analytical Methods in Food, Biological and Environmental Samples Determination II)

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15 pages, 1727 KiB

Open AccessReview

Detection Techniques for Lead Ions in Water: A Review

by Dan Wu, Yinglu Hu, Huan Cheng and Xingqian Ye

Molecules 2023, 28(8), 3601; https://doi.org/10.3390/molecules28083601 - 20 Apr 2023

Cited by 34 | Viewed by 5644

Abstract

Lead pollution has increasingly become the focus of environmental pollution, which is a great harm to the ecological environment and human health. Strict control of the emission of lead pollutants and accurate monitoring of lead are very important. The lead ion detection technologies are introduced here, including spectrophotometry, electrochemical method, atomic absorption spectrometry, and other detection methods, and the methods’ applicability, the advantages, and disadvantages are discussed. The detection limits of voltammetry and atomic absorption spectrometry are as low as 0.1 μg/L, and those of atomic absorption spectrometry are as low as 2 μg/L. The detection limit of photometry is higher (0.01 mg/L), but this method can be achieved in most laboratories. The application of different extraction pretreatment technologies in lead ion detection is introduced. The new technologies develop at home and abroad, such as precious metal nanogold technology, paper microfluidic technology, fluorescence molecular probe technology, spectroscopy, and other emerging technologies in recent years, are reviewed, and the principle and application of various technologies are expounded. Full article

(This article belongs to the Special Issue Development of Analytical Methods in Food, Biological and Environmental Samples Determination II)

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10 pages, 861 KiB

Open AccessBrief Report

A UPLC-MS/MS Based Rapid, Sensitive, and Non-Enzymatic Methodology for Quantitation of Dietary Isoflavones in Biological Fluids

by Faraz Rashid, Sudeep Ghimire, Ashutosh K. Mangalam and Shailendra Giri

Molecules 2023, 28(18), 6729; https://doi.org/10.3390/molecules28186729 - 21 Sep 2023

Cited by 1 | Viewed by 1459

Abstract

Dietary isoflavones, a type of phytoestrogens, have gained importance owing to their health-promoting benefits. However, the beneficial effects of isoflavones are mediated by smaller metabolites produced with the help of gut bacteria that are known to metabolize these phytoestrogenic compounds into Daidzein and Genistein and biologically active molecules such as S-Equol. Identifying and measuring these phytoestrogens and their metabolites is an important step towards understanding the significance of diet and gut microbiota in human health and diseases. We have overcome the reported difficulties in quantitation of these isoflavones and developed a simplified, sensitive, non-enzymatic, and sulfatases-free extraction methodology. We have subsequently used this method to quantify these metabolites in the urine of mice using UPLC-MS/MS. The extraction and quantitation method was validated for precision, linearity, accuracy, recoveries, limit of detection (LOD), and limit of quantification (LOQ). Linear calibration curves for Daidzein, Genistein, and S-Equol were set up by performing linear regression analysis and checked using the correlation coefficient (r² > 0.995). LOQs for Daidzein, Genistein, and S-Equol were 2, 4, and 2 ng/mL, respectively. This UPLC-MS/MS swift method is suitable for quantifying isoflavones and the microbial-derived metabolite S-Equol in mice urine and is particularly useful for large numbers of samples. Full article

(This article belongs to the Special Issue Development of Analytical Methods in Food, Biological and Environmental Samples Determination II)

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