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Table of Content

    22 December 2024, Volume 54 Issue 12 Previous Issue    Next Issue
    Basic research
    Performance of branched-chain extended surfactant mixed with zwitterionic or cationic surfactant
    Xiaoding Zeng, Yancheng Zheng, Guoqing Zhang, Lingchi Zeng, Jian Mu
    2024, 54 (12):  1405-1413.  doi: 10.3969/j.issn.2097-2806.2024.12.001
    Abstract ( 2157 )   HTML ( 14 )   PDF (6684KB) ( 67 )  

    2-Hexyl-1-decanol was used as the main material to prepare a block-polyether sulfonate extended surfactant (IC16P6E6S). The solubility and surface active properties of IC16P6E6S were evaluated, and then the IC16P6E6S was mixed with a cationic surfactant hexadecyl trimethyl ammonium bromide (CTAB) and a zwitterionic betaine surfactant (HAB), respectively. The effects of mixing ratios of IC16P6E6S∶HAB and IC16P6E6S∶CTAB on the hydrodynamic diameter and interfacial properties were discussed. The emulsification, adsorption and laboratory core displacement experiments of the binary system were tested. The results showed that the critical micelle concentration (cmc) of IC16P6E6S in distilled water was 0.1 mmol/L and the surface tension at cmc (γcmc) was 28.53 mN/m. IC16P6E6S showed strong synergistic effects with HAB and CTAB, and the mixed systems could effectively reduce the interfacial tension compared with single surfactants. The mixed systems with n (IC16P6E6S) ∶n (HAB) of 1∶1 and n (IC16P6E6S) ∶n(CTAB) of 1∶3 could maintain ultra-low interfacial tension (in the order of magnitude of 10-3 mN/m) in the salinity range of 1%-7% NaCl and low interfacial tension (in the order of magnitude of 10-2 mN/m) in the salinity range of 3%-7% NaCl, respectively. With the increase of salinity, the emulsion formed by the mixed surfactant system underwent the phase transition process from Winsor Ⅰ to Winsor Ⅲ and then to Winsor Ⅱ. The emulsion of mixed IC16P6E6S/HAB system had more middle-phase emulsion volume than that of the mixed IC16P6E6S/CTAB system, and the former emulsion system was more stable. The mixed IC16P6E6S/HAB system also had good solubilization effect, and the amount of oil solubilization was up to 43 mL/g. Meanwhile, it had good adsorption resistance. Compared with water flooding, the depressurization rate could reach 25.00% and the recovery could be enhanced by 11.75%, indicating that the IC16P6E6S/HAB system was more conducive to the depressurization and injection enhancement for low-permeability reservoirs.

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    Lecture of science and technology
    Preparation, properties and applications of natural biomass materials (Ⅻ) Multifunctional acidic heteropolysaccharide: pectin
    Yadi Liu, Kaiyue Guo, Axiu Gao, Yejie Zhou, Jinshi Fan
    2024, 54 (12):  1414-1422.  doi: 10.3969/j.issn.2097-2806.2024.12.002
    Abstract ( 1384 )   HTML ( 17 )   PDF (8209KB) ( 40 )  

    Pectin is a kind of natural hydrophilic colloid with complicated composition and structure, which has been abundantly found in the cells of higher plants. Pectin has good water solubility, stability, gelling ability and emulsifying ability, as well as safety and non-toxicity, good biocompatibility, biodegradability, and many excellent biological activities such as lowering cholesterol, anti-tumor, anti-oxidation, and lowering blood sugar. Moreover, both its physicochemical properties and functional performance can be further improved by physical, chemical and enzymatic treatments and compound modification upon the active functional groups, such as hydroxyl groups, carboxyl groups and glycosidic bonds. Therefore, pectin has been widely used in many fields, including food industry and pharmaceutical industry. Furthermore, great application potential has emerged in daily-use chemical industry, functional materials, and biodegradable biological materials. In this review, the source, chemical structure, main physicochemical properties and functional characteristics of pectin were briefly introduced. The extraction methods, separation and purification technologies, and modification methods for pectin were also systematically presented. In addition, the situation of application as well as the current problems for pectin and its modified products were summarized. Finally, some of the directions of future research and development of pectin were pointed out.

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    Development and application
    Coacervation of oxidized glutathione with a cationic surfactant and the application in dye removal
    Yue Zhang, Yu Liu, Li Zhao, Ce Wang, Baocai Xu
    2024, 54 (12):  1423-1430.  doi: 10.3969/j.issn.2097-2806.2024.12.003
    Abstract ( 1682 )   HTML ( 10 )   PDF (6082KB) ( 38 )  

    Coacervation of oxidized glutathione (GSSG) and a cationic surfactant, didodecyldimethylammonium bromide (DDAB), was constructed mainly driven by the electrostatic and hydrophobic interactions. The pH-dependent coacervate of GSSG-DDAB (1∶4, mol/mol) was analyzed. Under acidic and neutral conditions, a turbid suspension of droplets is observed, and alkaline pH results in the phase separation of coacervates as the top phase. The coacervate phase exhibits good performance (extraction efficiency>85%) in extracting several dyes from water, including brilliant yellow, acid red 13, cresyl violet acetate, eriochrom blue SE, and 4-hydroxyazobenzene. The dyes are added into the suspension in acidic conditions. Then, the dyes are enriched and extracted along with the coacervates as the top phase when pH is adjusted to~10. Coacervation of GSSG with DDAB provides a simple approach to extract organic pollutants in wastewater treatment.

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    Study on the growth of honeycomb-like film of basic zinc carbonate induced by bovine serum albumin LB film template
    Haiwei Wang, Wenbo Xiao, Xiuling Jia, Yang Xiao, Zuliang Du
    2024, 54 (12):  1431-1436.  doi: 10.3969/j.issn.2097-2806.2024.12.004
    Abstract ( 46 )   HTML ( 3 )   PDF (5612KB) ( 15 )  

    Honeycomb-like films of basic zinc carbonate were successfully prepared on FTO (SnO2: F) conductive glass using bovine serum albumin (BSA) as a template at room temperature. After low-temperature annealing, a high-specific-surface-area porous ZnO film with excellent electron mobility was obtained. The surface morphology, crystallization performance, and photoluminescence characteristics of basic zinc carbonate thin films and annealed ZnO thin film were analyzed by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), photoluminescence spectroscopy (PL) and UV-Visible spectroscopy (UV-vis). By comparing with those samples prepared without any protein, it was determined that the complexation between BSA molecules and Zn2+ ions was the primary factor in the synthesis of porous films of basic zinc carbonate. The experimental results showed that the ZnO thin film samples prepared with this method had high specific surface area and broadband luminescence characteristics in the near ultraviolet range.

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    Skin brightening benefit of 4-hexylresorcinol in vivo and in vitro and its underlying mechanism
    Xuelan Gu, Hong Zhang, Xue Xiao, Zhuang Zhou, Jue Qu, Yibing Shi
    2024, 54 (12):  1437-1446.  doi: 10.3969/j.issn.2097-2806.2024.12.005
    Abstract ( 2252 )   HTML ( 18 )   PDF (7450KB) ( 73 )  

    4-Hexylresorcinol (4-HR), a potent tyrosinase inhibitor, has been used as an even-tone active ingredient for skin care application since 2007. While the skin brightening efficacy of 4-HR in Chinese population has not been thoroughly investigated and its significance in keratinocytes has not been fully raveled. This study aims to evaluate the skin brightening potential of 4-HR in vivo and in vitro and explore its new mechanism of action through transcriptome approach. The skin brightening effect of 0.4% 4-HR in a facial serum was assessed in an 8-week, double-blinded, placebo-controlled, and randomized clinical study in 67 Chinese participants. ITA°, melanin index (MI) and visual grading were measured at baseline and 2, 4 and 8 weeks after use. A pigmented living skin equivalent (pLSE) model constructed from Asian skin cells was utilized to assess the brightening efficacy of 0.4% 4-HR by measuring the model’s brightness (L* value) and melanin content. Then, transcriptomic analysis of 4-HR treated human epidermal keratinocytes was conducted, and the two in vitro models were adopted for hypothesis validation afterwards. In the clinical study, the result shows both 0.4% 4-HR serum and placebo chassis can significantly improve all measures as compared to baseline at the 2, 4, and 8 weeks. Furthermore, 0.4% HR serum demonstrates a better performance in increasing ITA° as early as 2 weeks of application and decreasing MI value than the placebo group at Week 2. In the pLSE model, 0.4% 4-HR with topical application evidently increases L* value by 15.88% and decreases melanin content by 47.61% compared to UVB group. RNA-sequencing analysis implies that 4-HR can regulate multiple biological processes including skin development, keratinocyte differentiation, oxidant activity and autophagy function. In the blue-light challenged human keratinocytes model, 4-HR shows a significant ROS suppression capacity. In the keratinocytes-melanocytes co-culture model, 4-HR prompts autophagy activity and decreases melanin content. Most importantly, the melanin inhibitory activity of 4-HR is compromised after co-treating with Chloroquine, an autophagy inhibitor, suggesting autophagy regulation property of 4-HR may partially contribute to its skin brightening efficacy. Taken together, these data demonstrate skin brightening efficacy of 0.4% 4-HR in vivo and in vitro, in addition to acting as a tyrosinase inhibitor, 4-HR can contribute to skin brightening benefit via enhancing cellular antioxidant capacity and autophagy activation.

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    Study on the preparation and properties of sunscreen O/W/Si multiple emulsion
    Wanping Zhang, Lv Zhou, Zihao Gao, Haiyang Zhu
    2024, 54 (12):  1447-1455.  doi: 10.3969/j.issn.2097-2806.2024.12.006
    Abstract ( 112 )   HTML ( 11 )   PDF (7547KB) ( 64 )  

    To solve the greasiness and irritation risks brought about by organic sun-screening agents in sunscreen emulsions, in this work, a sunscreen O/W/Si multiple emulsion was prepared by two-step emulsification method, in which the outer oil phase was silicone oil and the inner oil phase was solid lipid nanoparticles coated with organic sun-screening agent. Several influencing factors on the formation and stability of the emulsion were analyzed, including inorganic salts, the volume fraction of outer oil phase (silicone oil), and the dosage of W/O emulsifier. The in vitro sunscreen performance, water resistance and skin permeability of different types of sunscreen emulsions were further studied. The results showed that the sunscreen O/W/Si multiple emulsion containing 22.5% silicone oil, 2.5% emulsifier and 0.2% NaCl had the best stability under the experimental conditions. The SPF value and water resistance of sunscreen O/W/Si multiple emulsion were slightly higher than those of sunscreen W/O emulsion, but significantly higher than those of sunscreen O/W emulsion. Compared with sunscreen W/O emulsion, the in vitro transdermal permeability of organic sun-screening agent in sunscreen O/W/Si multiple emulsion was reduced by approximately 60%, indicative of higher safety and good application prospect in sunscreen cosmetics.

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    Effect of fermented polypeptide of Sacha Inchi (Plukenetia volubilis L.) on the structure of liquid crystal emulsion
    Xiaochun Liu, Tingting Luo, Jie Dai, Laicheng Chen, Qiuxing He
    2024, 54 (12):  1456-1464.  doi: 10.3969/j.issn.2097-2806.2024.12.007
    Abstract ( 1729 )   HTML ( 9 )   PDF (7558KB) ( 34 )  

    In order to study the action mechanism of Sacha Inchi polypeptide in liquid crystal emulsion, oil-in-water liquid crystal emulsions with Sacha Inchi fermented polypeptide as the active component were prepared. The microstructures, particle sizes, stabilities, thermodynamic properties, and rheological properties of liquid crystal emulsions with different concentrations of the fermentation products were observed by Polarizing microscope, Particle size meter, Thermogravimetric differential thermal synchronous measurement system, and Rheometer, respectively. The results showed that the average particle size of fermented peptide liquid crystal emulsion was (25.7±2.8) μm, and the liquid crystal structure was complete and stable. The content of bound water and liquid crystal in the emulsion with 1% Sacha Inchi polypeptide were higher than those in the blank emulsion and the emulsions with 3% and 5% Sacha Inchi polypeptide. Rheological results indicated that the viscosity of liquid crystal emulsion with the change curve of shear rate registered the shear thinning phenomenon, which belongs to non-Newtonian fluid. The hysteresis area, energy storage modulus, and loss modulus of the 1% additive amount of liquid crystal emulsion were larger than those of the blank emulsion and the emulsions with 3% and 5% Sacha Inchi polypeptide, indicating greater thixotropy and stronger shear resistance. The hydrophilic amino acid residues of the peptide in the 1% additive amount of the emulsion were combined with the water phase, while the hydrophobic amino acid residues of the peptide entered the oil phase, which formed a viscoelastic film at the oil-water interface, so that the liquid crystal emulsion had a more stable gel network structure.

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    Preparation of Ce-TiO2-RGO catalyst and its application in the treatment of printing and dyeing wastewater
    Bao Zhu, Yan Pan
    2024, 54 (12):  1465-1472.  doi: 10.3969/j.issn.2097-2806.2024.12.008
    Abstract ( 42 )   HTML ( 6 )   PDF (6700KB) ( 18 )  

    Ce-TiO2-RGO composite photocatalyst was prepared by sol-gel method and ultrasonic treatment. The effect of Ce doping mass fraction on the degradation of textile printing and dyeing wastewater was studied. The catalysts were characterized by XRD, SEM, TEM, UV-vis and PL. The results showed that, Ce-TiO2 particles uniformly adsorbed on the GO surface, and the particle diameter of Ce-TiO2 was approximately 25-110 nm. After Ce doping, the absorption band edge of TiO2-RGO composite photocatalyst was redshifted and the band gap was reduced. With the increase of Ce doping mass fraction, the PL intensity of Ce-TiO2-RGO composite photocatalyst first decreased and then slightly increased, and the emission peak intensity of 6% Ce-TiO2-RGO composite photocatalyst was the lowest at 410 nm and 470 nm. Taking textile printing and dyeing wastewater as the research object of degradation, the COD removal rate of 6% Ce-TiO2-RGO reached the maximum of 82.21% at 180 min, and the COD value after degradation was 88.95 mg/L which was in line with the wastewater discharge standard. On the other hand, at 180 min, the degradation rate for textile printing and dyeing wastewater by 6% Ce-TiO2-RGO also reached the maximum (99.21%). Therefore, the Ce-TiO2-RGO composite photocatalyst showed great application potential in the treatment of textile dyeing wastewater.

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    Removal of ammonia nitrogen from inorganic wastewater by AgBr/C3N5 heterojunction under visible light irradiation
    Bingsheng Zhu
    2024, 54 (12):  1473-1480.  doi: 10.3969/j.issn.2097-2806.2024.12.009
    Abstract ( 37 )   HTML ( 3 )   PDF (5696KB) ( 12 )  

    AgBr/C3N5 composite was prepared by in-situ precipitation of AgBr on the surface of nitrogen-rich carbon nitride (C3N5). The crystal phase, chemical composition, elemental composition, spectral absorption and photoelectron-hole separation of the composite were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), ultraviolet-visible diffuse reflectance spectroscopy (UV-vis DRS) and photoluminescence spectroscopy (PL). The construction of AgBr and C3N5 heterojunction could broaden the spectral response range, realize the efficient separation of photoelectrons and holes, and thus improve the photocatalytic performance. The photocatalytic performance of the composite material was studied by simulating inorganic ammonia nitrogen wastewater with NH4Cl solution. The dosage of the composite material was 0.10 g, the initial mass concentration of NH4Cl solution was 100 mg/L, and the initial pH was 10.0. The removal rate of ammonia nitrogen by the composite material reached 90.27% after 60 min of simulated visible light irradiation. After 5 cycles, the removal rate of ammonia nitrogen only declined by 0.12%. The composite material showed good photocatalytic performance and stability. The Z-scheme mechanism effectively retained the reduction and oxidation activities of photoelectrons and holes, which could change O2 and H2O to active groups such as superoxide radicals (·O2-) and hydroxyl radicals (·OH), respectively, achieving efficient removal of inorganic ammonia nitrogen.

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    Study on the repairing effect of poly (N-vinylpyrrolidone-co-methacrylic acid) on permed or bleached damaged hair
    Yun Zhang, Huan Wang, Yuyun Yang, Sihan Yu, Yuhua Cao
    2024, 54 (12):  1481-1488.  doi: 10.3969/j.issn.2097-2806.2024.12.010
    Abstract ( 57 )   HTML ( 2 )   PDF (6335KB) ( 16 )  

    The repairing effect of poly (N-vinylpyrrolidone-co-methacrylic acid) on permed or bleached damaged hair was studied. The combing and tensile strength of permed and bleached hair before and after treatment with the copolymer solution were tested, and the effects of the mass fraction of copolymer solution and immerseing time on the combing and tensile strength for permed or bleached damaged hair were investigated. The repair mechanism of permed or bleached damaged hair was also explored. The results show that when the immersing time is 3 hours, the tensile strength of the permed hair increases with the mass fraction of the copolymer solution within 0%-0.3%, but no obvious change is observed when the mass fraction is over 0.3%. Therefore, the optimal mass fraction of the copolymer solution for repairing the permed hair is 0.3%. Similarly, the optimal mass fraction of the copolymer solution for repairing the bleached hair is 0.5%. Furthermore, the effects of immersing time on the tensile strength of the damaged hair fibers were compared between the permed and bleached hair before and after treatment with the copolymer solution. Coincidentally, the optimal immersion time for permed or bleached damaged hair is both 2 hours. The tensile strength of the permed and bleached hair soaked in 0.3% and 0.5% copolymer solutions for 2 hours increases by 15.55% and 18.12%, respectively, compared to untreated hair. Through infrared spectroscopy analysis, it is found that the amide II band in hair fibers shifted to the blue after repair, with the wave number shift of 11.12 and 11.09 cm-1, which confirm the formation of hydrogen bonds in the hair samples. Additionally, the urea hydrogen bond disruption experiment demonstrates that urea does not disrupt the hydrogen bonds in untreated hair fibers, but prevents the formation of new hydrogen bonds in damaged hair fibers. It further validates that the improvement of the tensile strength of the copolymer treated damaged hair fibers is mainly due to the formation of hydrogen bonds. After treatment with the copolymer, the dry and wet combing friction decrease by 30.73% and 28.55% for the permed hair, and decrease by 28.55% and 24.83% for the bleached hairs, respectively. The scanning electron microscope shows that the copolymer can flatten the cuticle and fill the space between the raised cuticles.

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    Reviews
    Research progress on the application of ferulic acid in cosmetics
    Shiyu Deng, Jianming Jin, Hua Wu
    2024, 54 (12):  1489-1496.  doi: 10.3969/j.issn.2097-2806.2024.12.011
    Abstract ( 2039 )   HTML ( 8 )   PDF (7103KB) ( 57 )  

    Ferulic acid is a phenolic compound widely exists in plants. Currently ferulic acid on the market is mainly extracted from plants, but it can also be obtained via biosynthesis or chemical synthesis. The biosynthesis method has a great potential for future production of ferulic acid. Ferulic acid is frequently used as a whitening ingredient in cosmetics, since it reduces melanin production by competitively inhibiting tyrosinase activity. It also has strong antioxidant activity, including elimination of free radicals, inhibition of ROS production, and regulation of various signaling pathways and the activity of antioxidant enzymes. The anti-UV activity of ferulic acid makes it applicable in sunscreen cosmetics. It can absorb UV rays and inhibit UVB-induced matrix metalloproteinase MMP-2 and MMP-9 activities to attenuate the damage caused by UV radiation. Ferulic acid is also reported to display protective effects on human keratinocytes and human skin fibroblasts. In addition, it is found to have effective anti-aging effect, mainly through inhibiting the degradation of hyaluronic acid by reducing the activities of collagenase and hyaluronidase, and inducing the biosynthesis of pre-collagen and hyaluronic acid. Ferulic acid shows potential for the treatment of atopic dermatitis, psoriasis and other inflammatory diseases of the skin. Its anti-inflammatory effect results from the inhibition of multiple inflammatory factors and signaling pathways. Ferulic acid displays broad-spectrum antibacterial effect, by damaging the cell membranes of bacteria and fungi which leads to membrane leakage and cell death. Furthermore, ferulic acid can also promote skin healing and regeneration. However, the instability of ferulic acid limits its applications in cosmetics.

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    Research progress on the skincare efficacy of sulfated glycosaminoglycans
    Yanwei Zhang, Zhongliang Xu, Xi Du, Zhen Li, Zhipeng Tian
    2024, 54 (12):  1497-1503.  doi: 10.3969/j.issn.2097-2806.2024.12.012
    Abstract ( 59 )   HTML ( 3 )   PDF (5966KB) ( 36 )  

    With the improvement of consumers’ scientific skin care consciousness, skin problems-oriented efficacy skin care and precise skin care methods have become the future development trend. Glycosaminoglycans are long, linear polysaccharides comprised of repeated disaccharide units, which are highly expressed endogenously in the skin. They are commonly present in skin cells, cell surface and extracellular matrix, with pleiotropic biological function. In addition to hyaluronic acid, the sulfated glycosaminoglycans heparin, heparan sulfate, dermatan sulfate and chondroitin sulfate play an important role in anti-wrinkle, firming, soothing, and improving microvascular circulation, but are still in the research and development stage in cosmetics. This paper summarizes the skincare mechanism of sulfated glycosaminoglycans, and demonstrates the potential of sulfated glycosaminoglycans as functional raw materials in cosmetics.

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    A review of methods for evaluating effectiveness of cosmetic products and ingredients based on mechanisms of the human hair growth cycle
    Jiaqi Zhang, Kening Wan, Ranjit Kaur Bhogal, Mingming Pu, Jiayin Gu, Yao Pan
    2024, 54 (12):  1504-1514.  doi: 10.3969/j.issn.2097-2806.2024.12.013
    Abstract ( 140 )   HTML ( 7 )   PDF (9295KB) ( 74 )  

    With the increasing incidence of hair loss and especially among younger population in recent years, the demand for diversified products on anti-hair loss solutions is growing and the market of cosmetic products expanding accordingly. Worldwide attention is being paid to the research and development of anti-hair loss actives, while there is no unified standard for the efficacy evaluation and testing methods of anti-hair loss cosmetics. Therefore, it is critical to establish standardized methodology for assessing the effectiveness of anti-hair loss actives and their cosmetic products. In this review, an overview of the human hair follicle structure, the hair follicle cycle, and the biological pathways and signaling mechanisms involved in hair growth are summarized. This provides the fundamental understanding of human hair growth for reviewing anti-hair loss actives and cosmetic hair loss products, and respective methods and techniques applied for evaluating their efficacy. Additionally, changes in the normal hair cycle, and corresponding cosmetic strategies to slow down and reduce hair loss have been provided. This review aims to provide recommendations for evaluating the effectiveness of anti-hair loss actives on the mechanisms involved in the hair follicle growth cycle, and so provide criteria for new technology development and scientific research for cosmetic products.

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    Analytical methods and testing
    Simultaneous determination of 27 preservatives in toothpaste by high-performance liquid chromatography
    Zhishan Wu, Yanchao Wang, Chengjun Jiang, Yuchen Long, Shuai Yin, Weicheng Yin
    2024, 54 (12):  1515-1523.  doi: 10.3969/j.issn.2097-2806.2024.12.014
    Abstract ( 56 )   HTML ( 5 )   PDF (4865KB) ( 28 )  

    A method of high-performance liquid chromatography (HPLC) was established for simultaneous determination of 27 preservatives in toothpaste. Toothpaste samples were extracted with 50% aqueous methanol solution, ultrasonicated and then filtered. The target compounds were separated on a C18 column (250 mm×4.6 μm, 5 μm) with the mobile phase consisting of acetonitrile and aqueous phosphoric acid solution, the column temperature was 30 ℃, the sample volume was 10 μL, the flow rate was 1 mL/min, and diode array detector was used. Under the optimal experimental conditions, good linear relationship was obtained and the correlation coefficient (R2) was greater than 0.999 5. This method was accurate and sensitive, which was suitable for the qualitative and quantitative analysis of 27 preservatives in toothpaste.

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    Research on the quality control technology for the Astragalus membranaceus extraction solution in cosmetics
    Rupei Wang, Liang Chu, Qingying Chen, Wenli Li, Chunyan Li, Ping Fu
    2024, 54 (12):  1524-1531.  doi: 10.3969/j.issn.2097-2806.2024.12.015
    Abstract ( 71 )   HTML ( 4 )   PDF (6221KB) ( 24 )  

    Calycosin-7-glucoside, which is the target ingredient of the Astragalus membranaceus extraction solution, was studied by the high-performance liquid chromatography-diode array detector method (HPLC-DAD), and a high-performance liquid chromatography-electrospray ionization detector method (HPLC-CAD) was also established for fingerprint chromatogram analysis. Meanwhile, the heavy metal content was tested to build a quality control standard for Astragalus membranaceus extraction solution. Result shows a good linearity in 4-80 μg/mL mass concentration range with the correlation coefficient r=0.999, RSD=2.4%, and the recovery rate is between 99.2%-102.7%. The fingerprint chromatogram analysis features with 14 specific peaks, including 5 identified components. The similarity is between 0.485 to 0.995. Content of heavy metals such as lead, mercury, and cadmium are below the detection limit, and the content of arsenic is less than 2 mg/kg. This research results can serve as process optimization basis and quality control standards for Astragalus membranaceus extraction solution, and provide reference to quality control and research guideline for other cosmetics using herbal extracts as raw materials.

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    Determination of 13 preservatives in cosmetics by high performance liquid chromatography and verification by mass spectrometry
    Po Zou, Wei Xu, Xueyan Li, Changyu Li, Yan Chen, Qinqin Chen
    2024, 54 (12):  1532-1540.  doi: 10.3969/j.issn.2097-2806.2024.12.016
    Abstract ( 169 )   HTML ( 4 )   PDF (6069KB) ( 30 )  

    A method using high performance liquid chromatography (HPLC) was developed for the simultaneous determination of 13 preservatives (levulinic acid, p-hydroxyacetophenone, raspberry ketone, p-anisic acid, caprylhydroxamic acid, hydroxyethoxyphenyl butanone, methylisothiazolinone, phenoxyethanol, benzoic acid, methylparaben, chlorphenesin, dehydroacetic acid, and 5-bromo-5-nitro-1,3-dioxane) in cosmetics. Different types of samples were ultrasonically extracted by methanol, then the separation of 13 preservatives was carried out on a column of Agilent ZORBAX Eclipse XDB-C18 (250 mm×4.6 mm, 5 μm) by gradient elution at a flow rate of 1.0 mL/min, using 0.1% phosphoric acid solution and acetonitrile as mobile phases. The column temperature was 30 ℃, and the detection was completed by a diode array detector with the wavelengths at 275, 230 and 210 nm. Suspected positive samples were further confirmed by liquid chromatography-tandem mass spectrometry or gas chromatography-mass spectrometry. The linear regression analysis data shows good linearity for 13 preservatives in the respective mass concentration range, with their correlation coefficients (r) greater than 0.999 8. The limits of detection (LODs) and limits of quantitation (LOQs) of the method are in the ranges of 0.4-100.0 mg/kg and 1.2-250.0 mg/kg, respectively. At three spiked levels, the average recoveries for 13 target compounds in three kinds of matrix samples are within 84.0%-115.4%, and the relative standard deviations (RSD) are within 0.5%-4.8% (n = 6). This method is convenient, efficient, and precise, which can be used for qualitative and quantitative analysis of common preservatives in daily cosmetics.

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