Progress in the analysis of phytocannabinoids by HPLC and UPLC (or UHPLC) during 2020-2023.

INTRODUCTION: Organic molecules that bind to cannabinoid receptors are known as cannabinoids. These molecules possess pharmacological properties similar to those produced by Cannabis sativa L. High-performance liquid chromatography (HPLC) and ultra-performance liquid chromatography (UPLC, also known as ultra-high-performance liquid chromatography, UHPLC) have become the most widely used analytical tools for detection and quantification of phytocannabinoids in various matrices. HPLC and UPLC (or UHPLC) are usually coupled to an ultraviolet (UV), photodiode array (PDA), or mass spectrometric (MS) detector. OBJECTIVE: To critically appraise the literature on the application of HPLC and UPLC (or UHPLC) methods for the analysis of phytocannabinoids published from January 2020 to December 2023. METHODOLOGY: An extensive literature search was conducted using Web of Science, PubMed, and Google Scholar and published materials including relevant books. In various combinations, using cannabinoid in all combinations, cannabis, hemp, hashish, C. sativa, marijuana, analysis, HPLC, UHPLC, UPLC, and quantitative, qualitative, and quality control were used as the keywords for the literature search. RESULTS: Several HPLC- and UPLC (or UHPLC)-based methods for the analysis of phytocannabinoids were reported. While simple HPLC-UV or HPLC-PDA-based methods were common, the use of HPLC-MS, HPLC-MS/MS, UPLC (or UHPLC)-PDA, UPLC (or UHPLC)-MS, and UPLC (or UHPLC)-MS/MS was also reported. Applications of mathematical and computational models for optimization of protocols were noted. Pre-analyses included various environmentally friendly extraction protocols. CONCLUSION: During the last 4 years, HPLC and UPLC (or UHPLC) remained the main analytical tools for phytocannabinoid analysis in different matrices.

In Vitro and In Vivo Anti-Aging Effect of Coffee Berry Nanoliposomes.

Encapsulation of bioactive compounds in the liposome system provides several advantages, such as enhancing the stability and lowering the toxicity of active compounds. Coffee berry extract (CBE) has previously been established to have in vitro anti-aging properties and to retard the aging of human skin. The purposes of this study were to encapsulate CBE in nanoliposomes and to assess its stability and in vitro anti-aging potential in human dermal fibroblasts (HDF), as well as in healthy human skin. In the HDF model, anti-aging potential was determined by nitric oxide (NO) and collagenase inhibition assays and a superoxide dismutase (SOD) activity assay, whereas in healthy human skin (in vivo), the skin elasticity and brightness were examined. First, liposomal CBE (L-CBE) was created with a particle size of 117.33 ± 2.91 nm, a polydispersity index (PDI) of 0.36 ± 0.03, and a zeta potential of -56.13 ± 1.87 mV. The percentages of encapsulation efficacy (%EE) and loading efficacy (%LE) were 71.26 ± 3.12% and 2.18 ± 0.18%, respectively. After undergoing a 12-week stability test, the L-CBE retained more phenolic content than the free CBE when stored at 4 °C, room temperature, and 45 °C. Compared to free CBE, the L-CBE demonstrated a more consistent, elevated, and prolonged release of phenolics from the lipid system. In human dermal fibroblasts, L-CBE showed lower toxicity, and at its maximum nontoxic concentration (10 mg/mL), it exhibited slightly higher anti-aging effects than CBE, including NO inhibition, enhanced SOD activity, and anti-collagenase activities. In clinical trials (30 volunteer subjects), none of the participants' skin was irritated when the L-CBE, the CBE, or base creams were applied. After 2 weeks of application, the L-CBE and CBE creams both demonstrated an improvement in skin elasticity and a reduction in melanin levels, and after 4 weeks, L-CBE cream showed a significantly greater improvement in skin elasticity and lightening. The results demonstrate that the encapsulation of the CBE in liposomal systems could increase its stability and skin penetration, reduce its toxicity, and maintain its anti-aging effect, which is powerful enough to be exploited in anti-aging and whitening agents for application in cosmetics and cosmeceuticals.

Simultaneous Extraction of Oil and Protein from Silkworm (Bombyx mori L.) Pupae (Lueng Parroj var.) and Their In Vitro Skin Moisturization.

Oil and protein from silkworm (Bombyx mori var. Leung Pairoj) pupae, by-product from sericulture, were extracted and evaluated for their potential uses as skin biomoisturizer. The silkworm pupae (SWP) oil and protein were simultaneously extracted by using three-phase partitioning (TPP) method and determined for their physicochemical properties including fatty acid and amino acid content, respectively. The highest yields of oil and protein at 8.24 ± 0.21% and 8.41 ± 0.26% w/w, respectively were obtained from 18 h extraction. Fatty acid analysis of SWP oil was rich in linolenic acid (37.81 ± 0.34%), oleic acid (28.97 ± 0.13%), palmitic acid (21.27 ± 0.05%), stearic acid (6.60 ± 0.09%) and linoleic acid (4.73 ± 0.21%). The clear yellow SWP oil possessed saponification value of 191.51 mg/g, iodine value of 119.37 g I2/g and peroxide value of 2.00 mg equivalent O2/kg. The SWP protein composed of 17 amino acids which aspartic acid, glutamic acid, glycine and serine were the major residues. SDS-PAGE analysis revealed that the SWP protein consisted of distinct protein at around 51, 70, 175 and over 175 kDa. Cytotoxicity of the SWP oil and protein was evaluated by using MTT assay and they showed low cytotoxicity toward keratinocyte cell (HaCat cell line). The SWP oil provided moisturizing effect on pig skin comparable to olive oil, while 1% and 2% of SWP protein showed higher moisturizing efficacy than 3% hydrolyzed collagen. The study indicated that the SWP oil and protein could be potential biomoisturizers for cosmetic products.

Utilization of Emulsion Inversion to Fabricate Tea (Camellia sinensis L.) Flower Extract Obtained by Supercritical Fluid Extraction-Loaded Nanoemulsions.

This study aimed to obtain tea flower extract (TFE) using supercritical fluid extraction, to determine the compounds present in the TFE and to establish its antioxidant activity. The fabrication of TFE nanoemulsions was also investigated using response surface methodology (RSM). UHPLC-ESI-QTOF-MS/MS and UHPLC-ESI-QqQ-MS/MS analysis showed that the TFE was composed of catechin and its derivatives, flavonols and anthocyanins, suggesting its potential as a free radical scavenger with strong reducing powers. A central composite design was applied to optimize the independent factors of the nanoemulsions. The factors had a significant (p < 0.05) effect on all response variables. The optimum level of factors for the fabrication was a surfactant-to-oil ratio of 2:1, a high hydrophilic-lipophilic balance (HLB) surfactant to low HLB surfactant ratio (HLR) of 1.6:1, and a PEG-40/PEG-60 hydrogenated castor oil ratio of 2:1. The responses obtained from the optimum levels were a 34.01 nm droplet size, a polydispersity index of 0.15, and 75.85% entrapment efficiency. In conclusion, TFE could be an antioxidant active ingredient and has been successfully loaded into nanoemulsions using RSM.

Chemical Constituents, Antioxidant, Anti-Tyrosinase, Cytotoxicity, and Anti-Melanogenesis Activities of Etlingera elatior (Jack) Leaf Essential Oils.

Essential oils of plants have been used widely in cosmetic preparations. Being both perfuming and active ingredients, the functions of essential oils mean they are high-value ingredients. In this study, the leaf of Etlingera elatior (Jack) or Torch ginger was used. The essential oils (EO) were prepared by conventional hydrodistillation (HD) and microwave-assisted hydrodistillation (MAHD). The volatile compounds of EOs were analyzed by gas chromatography spectroscopy (GC-MS). The antioxidant activities by means of DPPH radical scavenging and ferric-reducing antioxidant power (FRAP) were determined. The inhibition of tyrosinase activity was investigated. The cytotoxicity was performed against human fibroblast cell lines (NIH/3T3) and melanoma cell lines (A375 and B16F10). The decreasing melanin content was measured in melanoma cell lines. The resulting essential oils were detected for 41 compounds from HD extraction dominants by terpenes, namely sesquiterpenes (48.499%) and monoterpenes (19.419%), while 26 compounds were detected from MAHD with the fatty alcohols as the major group. The higher antioxidant activities were found in HD EO (IC50 of 16.25 ± 0.09 mg/mL from DPPH assay and 0.91 ± 0.01 mg TEAC/g extract from FRAP assay). The survival of normal fibroblast cell lines remained at 90% at 500 µg/mL HD EO, where the EO possessed the half-maximal toxicity dose (TD50) of 214.85 ± 4.647 and 241.128 ± 2.134 µg/mL on B16F10 and A375 cell lines, respectively. This could suggest that the EO is highly selective against the melanoma cell lines. The melanin content was decreased at the half-maximum efficacy (IC50) at 252.12 ± 3.02 and 253.56 ± 3.65 in the A375 and B1610 cell lines, respectively, which were approximately 2.8-fold lower than kojic acid, the standard compound. The results of this study evidence the use of Etlingera elatior (Jack) leaf as a source of essential oil as an active agent in cosmetics.

Polysaccharides from Volvariella volvacea Mushroom: Extraction, Biological Activities and Cosmetic Efficacy.

Polysaccharides from Volvariella volvacea (VVP) were investigated for their cosmetic-related activities and in vivo efficacy for use as a multifunctional active cosmetic ingredient. Three different polysaccharide extraction methods, including hot water shaking (HS), microwave-assisted (MA) and ultrasonic-assisted (UA), were used. Extractable yield, polysaccharide contents and biological activities, including antioxidant, anti-tyrosinase and anti-elastase activities, were compared. The polysaccharides from HS provided the highest extraction yield (15.58 ± 0.96% w/w) and the highest beta-glucan content (18.80 ± 0.81% w/w). The HS polysaccharides also possessed the highest inhibitory effects toward lipid peroxidation (IC50 of 0.0378 mg/mL), tyrosinase (51.46 mg KAE/g), and elastase (604.21 ± 73.66 mg EGCG/g). The cytotoxicity of the VVP was determined for safe use. A cosmetic gel cream containing VVP was developed and 0.2% VVP formulation was observed to be the most stable in color. UV protection factors, skin irritation by single patch test, and in vivo efficacy, including skin moisturization, anti-wrinkle and whitening, were measured. The VVP showed no cytotoxicity against human dermal skin fibroblast. The gel cream containing VVP provided less sun protection factor; however, it significantly exhibited the skin benefits of increasing moisture, gross elasticity, net elasticity, and skin firmness. Improvements to skin roughness, scaliness, wrinkles and in melanin content were also depicted gradually along 8 weeks. V. volvacea, therefore, could be a good source for polysaccharides being used as a moisturizing, anti-wrinkle, and whitening agent in cosmetic preparations.

The Feasibility of Utilizing Cultured Cordyceps militaris Residues in Cosmetics: Biological Activity Assessment of Their Crude Extracts.

Solid-based residues (SBRs) left from harvesting the fruiting bodies of cultured Cordyceps mushrooms are a challenge to sustainability. Therefore, in this study, the SBRs from the cultivation of Cordyceps militaris (C. militaris) via solid-state fermentation (SSF) were employed to prepare crude extracts, with the aim of considering their possible use in cosmetics. The SBRs obtained from cultivation with solid media containing defatted rice bran mixed with barley, white rice, Riceberry rice, and wheat were named SBR-B, SBR-R, SBR-Rb, and SRB-W, respectively. They were extracted with solvents of differing polarity and then evaluated for their total phenolic content (TPC), total flavonoid content (TFC), and total carbohydrate content (TCC). In addition, antioxidant and tyrosinase inhibitory activities, photoprotection, and cytotoxicity were also assessed. The results revealed that the total bioactive contents and biological capacities of crude SBR extracts were significantly influenced by the types of SBR and extraction solvent (p < 0.05). The SBR-B extracted with hot water exhibited the highest antioxidant activity (66.62 ± 2.10, 212.00 ± 3.43, and 101.62 ± 4.42 mg TEAC/g extract) when assayed by DPPH, ABTS, and FRAP methods, respectively, whereas tyrosinase inhibitory activity (51.13 ± 1.11 mg KAE/g extract) with 90.43 ± 1.96% inhibition at 1 mg/mL was excellently achieved by SBR-Rb extracted by 50% (v/v) ethanol. Correlations between bioactive contents in the crude extracts and their biological activities were mostly proven at a strong level (p < 0.01). The capability of the crude extracts to absorb UV over the range of 290-330 nm disclosed their potential roles as natural UV absorbers and boosters. Cytotoxicity analysis using fibroblast cell lines tested with hot water and 50% (v/v) ethanolic SBR extracts demonstrated safe use within a concentration range of 0.001-10 mg/mL. Interestingly, their fibroblast proliferative capacity, indicating anti-aging properties, was highly promoted. The chemical composition analyzed via LC-MS/MS techniques showed that seven phenolic acids and four flavonoids were identified in the crude SBR extracts. Furthermore, the other compounds present included nucleosides, nucleobases, amino acids, sugars, phospholipids, alkaloids, organic acids, vitamins, and peptides. Therefore, it is emphasized that SBRs from C. militaris can be a prospective source for preparing crude extracts employed in cosmetics. Lastly, they could be further utilized as multifunctional ingredients in cosmetics and cosmeceuticals.