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A special issue of Molecules (ISSN 1420-3049). This special issue belongs to the section "Flavours and Fragrances".

Deadline for manuscript submissions: closed (30 June 2022) | Viewed by 44485

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Dr. Maria Celeiro

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Department of Analytical Chemistry, Nutrition and Bromatology, University of Santiago de Compostela, Santiago de Compostela, Spain
Interests: bioactive compounds; chromatography; green sample preparation; mass spectrometry; characterization; added-value products; cosmetics
Special Issues, Collections and Topics in MDPI journals

Prof. Dr. Maria Llompart

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CRETUS Institute, Department of Analytical Chemistry, Nutrition and Food Science, Universidade de Santiago de Compostela, E-15782 Santiago de Compostela, Spain
Interests: sample preparation; extraction and microextraction; GC/MS; LC/MS; method development and validation; chemometrics; environmental pollutants; emerging contaminants; personal care products
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

The use of cosmetics and personal care products is increasing worldwide. They are complex matrices formed by a broad range of chemical compounds including classical ingredients such as fragrances, preservatives, UV filters or dyes, among others. However, in recent years, the trend has been moving toward including other additives such as bioactive molecules or compounds with nutraceuticals properties. Their matrix complexity, together with the wide range of cosmetics and personal care products currently marketed, imply a challenge for their analysis, with most of them requiring a sample pre-treatment step before analysis.

I cordially invite authors to contribute original articles or reviews that will give the readers of Molecules updated information about the recent advances in cosmetics and personal care products analysis. Such contributions may include new sample preparation strategies based on microextraction and green miniaturized techniques to determine a broad spectrum of compounds in cosmetic and personal care products, as well as the identification and characterization of bioactive compounds from natural plant extracts that could be employed as value-added ingredients.

This Special Issue is supported by the Sample Preparation Study Group and Network, supported by the Division of Analytical Chemistry of the European Chemical Society (https://www.sampleprep.tuc.gr/en/home/).

Dr. Maria Celeiro
Prof. Dr. Maria Llompart
Guest Editors

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Keywords

Cosmetic analysis
Personal care products
Green chemistry
Sample preparation
Microextraction techniques
Chromatographic analysis

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Last Advances in Cosmetics and Personal Care Products Analysis, 2nd Edition in Molecules (1 article)

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Research

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14 pages, 2387 KiB

Open AccessArticle

Validation of a High-Performance Liquid Chromatography with Photodiode Array Detection Method for the Separation and Quantification of Antioxidant and Skin Anti-Aging Flavonoids from Nelumbo nucifera Gaertn. Stamen Extract

by Duangjai Tungmunnithum, Samantha Drouet and Christophe Hano

Molecules 2022, 27(3), 1102; https://doi.org/10.3390/molecules27031102 - 7 Feb 2022

Cited by 14 | Viewed by 3820

Abstract

Nelumbo nucifera Gaertn., or the so-called sacred lotus, is a useful aquatic plant in the Nelumbonaceae family that has long been used to prepare teas, traditional medicines as well as foods. Many studies reported on the phytochemicals and biological activities of its leaves and seeds. However, to date, only few studies were conducted on its stamen, which is the most important ingredient for herbal medicines, teas and other phytopharmaceutical products. Thus, this present study focuses on the following: (1) the application of high-performance liquid chromatography with photodiode array detection for a validated separation and quantification of flavonoids from stamen; (2) the Nelumbo nucifera stamen’s in vitro and in cellulo antioxidant activities; as well as (3) its potential regarding the inhibition of skin aging enzymes for cosmetic applications. The optimal separation of the main flavonoids from the stamen ethanolic extract was effectively achieved using a core-shell column. The results indicated that stamen ethanolic extract has higher concentration of in vitro and in cellulo antioxidant flavonoids than other floral components. Stamen ethanolic extract showed the highest protective effect against reactive oxygen/nitrogen species formation, as confirmed by cellular antioxidant assay using a yeast model. The evaluation of potential skin anti-aging action showed that the stamen extract has higher potential to inhibit tyrosinase and collagenase compared with its whole flower. These current findings are the first report to suggest the possibility to employ N. nucifera stamen ethanolic extract as a tyrosinase and collagenase inhibitor in cosmetic applications, as well as the utility of the current separation method. Full article

(This article belongs to the Special Issue Last Advances in Cosmetics and Personal Care Products Analysis)

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21 pages, 8808 KiB

Open AccessArticle

Green Extraction of Antioxidant Flavonoids from Pigeon Pea (Cajanus cajan (L.) Millsp.) Seeds and Its Antioxidant Potentials Using Ultrasound-Assisted Methodology

by Duangjai Tungmunnithum, Samantha Drouet, Jose Manuel Lorenzo and Christophe Hano

Molecules 2021, 26(24), 7557; https://doi.org/10.3390/molecules26247557 - 13 Dec 2021

Cited by 18 | Viewed by 4865

Abstract

Pigeon pea is an important pea species in the Fabaceae family that has long been used for food, cosmetic, and other phytopharmaceutical applications. Its seed is reported as a rich source of antioxidants and anti-inflammatory flavonoids, especially isoflavones, i.e., cajanin, cajanol, daidzein, and genistein. In today’s era of green chemistry and green cosmetic development, the development and optimization of extraction techniques is increasing employed by the industrial sectors to provide environmentally friendly products for their customers. Surprisingly, there is no research report on improving the extraction of these isoflavonoids from pigeon pea seeds. In this present study, ultrasound-assisted extraction (USAE) methodology, which is a green extraction that provides a shorter extraction time and consumes less solvent, was optimized and compared with the conventional methods. The multivariate strategy, the Behnken–Box design (BBD) combined with response surface methodology, was employed to determine the best extraction conditions for this USAE utilizing ethanol as green solvent. Not only in vitro but also cellular antioxidant activities were evaluated using different assays and approaches. The results indicated that USAE provided a substantial gain of ca 70% in the (iso)flavonoids extracted and the biological antioxidant activities were preserved, compared to the conventional method. The best extraction conditions were 39.19 min with a frequency of 29.96 kHz and 63.81% (v/v) aqueous ethanol. Both the antioxidant and anti-aging potentials of the extract were obtained under optimal USAE at a cellular level using yeast as a model, resulting in lower levels of malondialdehyde. These results demonstrated that the extract can act as an effective activator of the cell longevity protein (SIR2/SIRT1) and cell membrane protector against oxidative stress. This finding supports the potential of pigeon pea seeds and USAE methodology to gain potential antioxidant and anti-aging (iso)flavonoids-rich sources for the cosmetic and phytopharmaceutical sectors. Full article

(This article belongs to the Special Issue Last Advances in Cosmetics and Personal Care Products Analysis)

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17 pages, 1942 KiB

Open AccessArticle

Application of Blue Honeysuckle Powder Obtained by an Innovative Method of Low-Temperature Drying in Skincare Face Masks

by Emilia Klimaszewska, Malgorzata Zieba, Klaudia Gregorczyk and Leszek Markuszewski

Molecules 2021, 26(23), 7184; https://doi.org/10.3390/molecules26237184 - 26 Nov 2021

Cited by 5 | Viewed by 3164

Abstract

Traditional technologies applied for obtaining plant raw materials for cosmetic production are based primarily on high-level processing, which is reflected in the qualitative composition of the resulting materials. By using low-temperature drying, it is possible to retain in the raw materials a range of valuable ingredients. In this study, blue honeysuckle powder was used as an ingredient of cosmetic face masks. The stability of the masks was evaluated. Dynamic viscosity, yield point and texture analysis of the cosmetics was performed. The color of the emulsions and the level of skin hydration after face mask application was determined. Emulsions were found to be stable. A decrease in dynamic viscosity of the emulsions as a function of increasing concentrations of the additive and under the conditions of rising rotational speed were observed. Similarly, an increase in the concentration of blue honeysuckle in the emulsions resulted in a decrease in the value of the yield point. Based on the results, it can be stated that the addition of blue honeysuckle caused a decrease in hardness of the masks, while the opposite trend was observed for adhesive force. It was found that an increase in the concentration of blue honeysuckle gave a reddish-yellow color to the samples. Corneometric assessment confirmed proper skin hydration after the application of the emulsions. Full article

(This article belongs to the Special Issue Last Advances in Cosmetics and Personal Care Products Analysis)

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12 pages, 1667 KiB

Open AccessArticle

Biogenic Silver Nanoparticles from Iris tuberosa as Potential Preservative in Cosmetic Products

by Maria Mondéjar-López, Alberto José López-Jiménez, Minerva Abad-Jordá, Angela Rubio-Moraga, Oussama Ahrazem, Loudes Gómez-Gómez and Enrique Niza

Molecules 2021, 26(15), 4696; https://doi.org/10.3390/molecules26154696 - 3 Aug 2021

Cited by 16 | Viewed by 3556

Abstract

Biogenic-silver nanoparticles emerge as new nanosilver platforms that allow us to obtain silver nanoparticles via “green chemistry”. In our study, biogenic-silver nanoparticles were obtained from Iris tuberosa leaf extract. Nanoparticles were characterized by a UV-vis spectroscopy, dynamical light scattering technique. The transmission electron microscope revealed spheric and irregular nanoparticles with 5 to 50 nm in diameter. Antimicrobial properties were evaluated against typical microbial contaminants found in cosmetic products, showing high antimicrobial properties. Furthermore, natural moisturizing cream was formulated with biogenic-silver nanoparticles to evaluate the preservative efficiency through a challenge test, indicating its promising use as preservative in cosmetics. Full article

(This article belongs to the Special Issue Last Advances in Cosmetics and Personal Care Products Analysis)

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14 pages, 4201 KiB

Open AccessArticle

Novel Spray Dried Algae-Rosemary Particles Attenuate Pollution-Induced Skin Damage

by Roberta Hoskin, Erika Pambianchi, Alessandra Pecorelli, Mary Grace, Jean-Philippe Therrien, Giuseppe Valacchi and Mary Ann Lila

Molecules 2021, 26(13), 3781; https://doi.org/10.3390/molecules26133781 - 22 Jun 2021

Cited by 14 | Viewed by 3015

Abstract

The present study investigated the effect of spray-dried algae-rosemary particles against pollution-induced damage using ex-vivo human biopsies exposed to diesel engine exhaust (DEE). For this, the complexation of hydroalcoholic rosemary extract with Chlorella (RCH) and Spirulina (RSP) protein powders was conducted. The process efficiency and concentration of rosmarinic acid (RA), carnosic acid (CA), and carnosol (CR) phenolic compounds of both products were compared. The RSP spray-dried production was more efficient, and RSP particles presented higher CR and CA and similar RA concentrations. Therefore, spray-dried RSP particles were prioritized for the preparation of a gel formulation that was investigated for its ability to mitigate pollution-induced skin oxinflammatory responses. Taken altogether, our ex-vivo data clearly demonstrated the ability of RSP gel to prevent an oxinflammatory phenomenon in cutaneous tissue by decreasing the levels of 4-hydroxynonenal protein adducts (4HNE-PA) and active matrix metalloproteinase-9 (MMP-9) as well as by limiting the loss of filaggrin induced by DEE exposure. Our results suggest that the topical application of spirulina-rosemary gel is a good approach to prevent pollution-induced skin aging/damage. Full article

(This article belongs to the Special Issue Last Advances in Cosmetics and Personal Care Products Analysis)

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14 pages, 1878 KiB

Open AccessArticle

Potentiometric Surfactant Sensor Based on 1,3-Dihexadecyl-1H-benzo[d]imidazol-3-ium for Anionic Surfactants in Detergents and Household Care Products

by Nikola Sakač, Dubravka Madunić-Čačić, Dean Marković, Lucija Hok, Robert Vianello, Bojan Šarkanj, Bojan Đurin, Krunoslav Hajdek, Božo Smoljan, Stjepan Milardović, Brunislav Matasović and Marija Jozanović

Molecules 2021, 26(12), 3627; https://doi.org/10.3390/molecules26123627 - 14 Jun 2021

Cited by 8 | Viewed by 3076

Abstract

A 1,3-dihexadecyl-1H-benzo[d]imidazol-3-ium-tetraphenylborate (DHBI-TPB) ion-pair implemented in DHBI-TPB surfactant sensor was used for the potentiometric quantification of anionic surfactants in detergents and commercial household care products. The DHBI-TPB ion-pair was characterized by FTIR spectroscopy and computational analysis which revealed a crucial contribution of the C–H∙∙∙π contacts for the optimal complex formation. The DHBI-TPB sensor potentiometric response showed excellent analytical properties and Nernstian slope for SDS (60.1 mV/decade) with LOD 3.2 × 10⁻⁷ M; and DBS (58.4 mV/decade) with LOD 6.1 × 10⁻⁷ M was obtained. The sensor possesses exceptional resistance to different organic and inorganic interferences in broad pH (2–10) range. DMIC used as a titrant demonstrated superior analytical performances for potentiometric titrations of SDS, compared to other tested cationic surfactants (DMIC > CTAB > CPC > Hyamine 1622). The combination of DHBI-TPB sensor and DMIC was successfully employed to perform titrations of the highly soluble alkane sulfonate homologues. Nonionic surfactants (increased concentration and number of EO groups) had a negative impact on anionic surfactant titration curves and a signal change. The DHBI-TPB sensor was effectively employed for the determination of technical grade anionic surfactants presenting the recoveries from 99.5 to 101.3%. The sensor was applied on twelve powered samples as well as liquid-gel and handwashing home care detergents containing anionic surfactants. The obtained results showed good agreement compared to the outcomes measured by ISE surfactant sensor and a two-phase titration method. The developed DHBI-TPB surfactant sensor could be used for quality control in industry and has great potential in environmental monitoring. Full article

(This article belongs to the Special Issue Last Advances in Cosmetics and Personal Care Products Analysis)

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17 pages, 5308 KiB

Open AccessArticle

Activity of Experimental Mouthwashes and Gels Containing DNA-RNA and Bioactive Molecules against the Oxidative Stress of Oral Soft Tissues: The Importance of Formulations. A Bioreactor-Based Reconstituted Human Oral Epithelium Model

by Andrei C. Ionescu, Elena Vezzoli, Vincenzo Conte, Patrizia Sartori, Patrizia Procacci and Eugenio Brambilla

Molecules 2021, 26(10), 2976; https://doi.org/10.3390/molecules26102976 - 17 May 2021

Cited by 2 | Viewed by 2668

Abstract

Background: DNA-RNA compounds have shown promising protection against cell oxidative stress. This study aimed to assess the cytotoxicity, protective, or preventive effect of different experimental formulations on oral epithelia’s oxidative stress in vitro. Methods: Reconstituted human oral epithelia (RHOE) were grown air-lifted in a continuous-flow bioreactor. Mouthwashes and gels containing DNA-RNA compounds and other bioactive molecules were tested on a model of oxidative stress generated by hydrogen peroxide treatment. Epithelia viability was evaluated using a biochemical MTT-based assay and confocal microscopy; structural and ultrastructural morphology was evaluated by light microscopy and TEM. Results: DNA-RNA showed non-cytotoxic activity and effectively protected against oxidative stress, but did not help in its prevention. Gel formulations did not express adequate activity compared to the mouthwashes. Excipients played a fundamental role in enhancing or even decreasing the bioactive molecules’ effect. Conclusion: A mouthwash formulation with hydrolyzed DNA-RNA effectively protected against oxidative stress without additional enhancement by other bioactive molecules. Active compounds, such as hyaluronic acid, β-Glucan, allantoin, bisabolol, ruscogenin, and essential oils, showed a protective effect against oxidative stress, which was not synergistic with the one of DNA-RNA. Incorporation of surfactant agents showed a reduced, yet significant, cytotoxic effect. Full article

(This article belongs to the Special Issue Last Advances in Cosmetics and Personal Care Products Analysis)

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12 pages, 1164 KiB

Open AccessArticle

Multi-Target Strategy to Uncover Unexpected Compounds in Rinse-Off and Leave-On Cosmetics

by Maria Celeiro, Laura Rubio, Carmen Garcia-Jares and Marta Lores

Molecules 2021, 26(9), 2504; https://doi.org/10.3390/molecules26092504 - 25 Apr 2021

Cited by 4 | Viewed by 3696

Abstract

The wide range and complexity of cosmetic formulations currently available on the market poses a challenge from an analytical point of view. In addition, during cosmetics manufacture, impurities coming from raw materials or formed by reaction of different organic compounds present in the formulation may be present. Their identification is mandatory to assure product quality and consumer health. In this work, micro-matrix solid-phase dispersion (μMSPD) is proposed as a multi-target sample preparation strategy to analyze a wide number of unexpected families of compounds including polycyclic aromatic hydrocarbons (PAHs), pesticides, plasticizers, nitrosamines, alkylphenols (APs), and alkylphenol ethoxylates (APEOs). Analytical determination was performed by gas chromatography-mass spectrometry (GC-MS) for the determination of 51 target compounds in a single run, whereas liquid chromatography tandem mass spectrometry (LC-MS/MS) was employed for the analysis of six APs and APEOs. Both methodologies were successfully validated in terms of linearity, accuracy, and precision in leave-on and rinse-off cosmetics. Limits of detection (LODs) were calculated in the low ng g⁻¹, showing their suitability to determine trace levels of impurities and banned compounds with different chemical natures, providing useful tools to cosmetic control laboratories and companies. Full article

(This article belongs to the Special Issue Last Advances in Cosmetics and Personal Care Products Analysis)

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17 pages, 3952 KiB

Open AccessArticle

Retaining Skin Barrier Function Properties of the Stratum Corneum with Components of the Natural Moisturizing Factor—A Randomized, Placebo-Controlled Double-Blind In Vivo Study

by Johannes Schleusener, Andrew Salazar, Jörg von Hagen, Jürgen Lademann and Maxim E. Darvin

Molecules 2021, 26(6), 1649; https://doi.org/10.3390/molecules26061649 - 16 Mar 2021

Cited by 13 | Viewed by 4002

Abstract

The influence of a topically applied formulation containing components of natural moisturizing factor (NMF) on barrier-related parameters of the stratum corneum (SC) was investigated in vivo using confocal Raman microspectroscopy in a randomized, placebo-controlled double-blind study on 12 volunteers for 14 days. This method allowed for the elucidation of subtle differences between the verum and the placebo even though the components of the verum naturally occur in the SC. This differentiation is not possible non-invasively by conventional methods. In this study, we found that the applied verum and placebo formulations disrupted the equilibrium of water, NMF and lipids in the SC. The adverse effects of the formulation could be mitigated by incorporating it into a simplified supplementation of NMF molecules. As a long-term effect, the amount of strongly bound water increases at 30–40% SC depth (p < 0.05) and the amount of weakly bound water decreases at 30–40% SC depth (p < 0.05) for the verum. This supplement was also unexpectedly able to prevent intercellular lipids (ICL) disorganization in selected depths. In the long term, the verum treatment limited the lateral disorganization of the ICL to the upper 20% SC depth. Further research is required to elucidate the interplay of these factors in the SC, to better understand their contribution to the equilibrium and barrier function of the skin. This understanding of the interaction of these naturally occurring components could help in the future to develop and optimize topical treatments for diseases like psoriasis, atopic dermatitis, ichthyosis where the skin barrier is disrupted. Full article

(This article belongs to the Special Issue Last Advances in Cosmetics and Personal Care Products Analysis)

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16 pages, 1658 KiB

Open AccessArticle

Direct Potentiometric Study of Cationic and Nonionic Surfactants in Disinfectants and Personal Care Products by New Surfactant Sensor Based on 1,3-Dihexadecyl−1H-benzo[d]imidazol−3-ium

by Nikola Sakač, Dean Marković, Bojan Šarkanj, Dubravka Madunić-Čačić, Krunoslav Hajdek, Božo Smoljan and Marija Jozanović

Molecules 2021, 26(5), 1366; https://doi.org/10.3390/molecules26051366 - 4 Mar 2021

Cited by 12 | Viewed by 2750

Abstract

A novel, simple, low-cost, and user-friendly potentiometric surfactant sensor based on the new 1,3-dihexadecyl−1H-benzo[d]imidazol−3-ium-tetraphenylborate (DHBI–TPB) ion-pair for the detection of cationic surfactants in personal care products and disinfectants is presented here. The new cationic surfactant DHBI-Br was successfully synthesized and characterized by nuclear magnetic resonance (NMR), Fourier transform infrared (FTIR) spectrometry, liquid chromatography–mass spectrometry (LC–MS) and elemental analysis and was further employed for DHBI–TPB ion-pair preparation. The sensor gave excellent response characteristics for CTAB, CPC and Hyamine with a Nernstian slope (57.1 to 59.1 mV/decade) whereas the lowest limit of detection (LOD) value was measured for CTAB (0.3 × 10⁻⁶ M). The sensor exhibited a fast dynamic response to dodecyl sulfate (DDS) and TPB. High sensor performances stayed intact regardless of the employment of inorganic and organic cations and in a broad pH range (2−11). Titration of cationic and etoxylated (EO)-nonionic surfactant (NSs) (in Ba²⁺) mixtures with TPB revealed the first inflexion point for a cationic surfactant and the second for an EO-nonionic surfactant. The increased concentration of EO-nonionic surfactants and the number of EO groups had a negative influence on titration curves and signal change. The sensor was successfully applied for the quantification of technical-grade cationic surfactants and in 12 personal care products and disinfectants. The results showed good agreement with the measurements obtained by a commercial surfactant sensor and by a two-phase titration. A good recovery for the standard addition method (98–102%) was observed. Full article

(This article belongs to the Special Issue Last Advances in Cosmetics and Personal Care Products Analysis)

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Review

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31 pages, 1024 KiB

Open AccessReview

Recent Advances in Sample Preparation for Cosmetics and Personal Care Products Analysis

by Maria Celeiro, Carmen Garcia-Jares, Maria Llompart and Marta Lores

Molecules 2021, 26(16), 4900; https://doi.org/10.3390/molecules26164900 - 13 Aug 2021

Cited by 31 | Viewed by 7777

Abstract

The use of cosmetics and personal care products is increasing worldwide. Their high matrix complexity, together with the wide range of products currently marketed under different forms imply a challenge for their analysis, most of them requiring a sample pre-treatment step before analysis. Classical sample preparation methodologies involve large amounts of organic solvents as well as multiple steps resulting in large time consumption. Therefore, in recent years, the trends have been moved towards the development of simple, sustainable, and environmentally friendly methodologies in two ways: (i) the miniaturization of conventional procedures allowing a reduction in the consumption of solvents and reagents; and (ii) the development and application of sorbent- and liquid-based microextraction technologies to obtain a high analyte enrichment, avoiding or significantly reducing the use of organic solvents. This review provides an overview of analytical methodology during the last ten years, placing special emphasis on sample preparation to analyse cosmetics and personal care products. The use of liquid–liquid and solid–liquid extraction (LLE, SLE), ultrasound-assisted extraction (UAE), solid-phase extraction (SPE), pressurized liquid extraction (PLE), matrix solid-phase extraction (MSPD), and liquid- and sorbent-based microextraction techniques will be reviewed. The most recent advances and future trends including the development of new materials and green solvents will be also addressed. Full article

(This article belongs to the Special Issue Last Advances in Cosmetics and Personal Care Products Analysis)

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