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Table of Content

    22 March 2022, Volume 52 Issue 3 Previous Issue    Next Issue
    Basic research
    Study on the Pickering emulsion stabilized by Alg@TiO2 microspheres for sunscreen formulation
    Xie Xin,Wang Weihao,Liu Huanyu,Sun Mengmeng,Li Qinyuan,Jia Lufan,Meng Tao
    2022, 52 (3):  229-236.  doi: 10.3969/j.issn.1001-1803.2022.03.001
    Abstract ( 400 )   HTML ( 114 )   PDF (1475KB) ( 332 )  

    Sunscreen products can reduce the damage caused by UV rays, reducing tanning, inflammation and skin cancer. However, chemical sunscreen is more toxic, and the existing physical sunscreen is not stable and has poor sunscreening effect. Therefore, the development of a sunscreen formula with sunscreen function and emulsion stability has attracted extensive attention. In this work, a Pickering emulsion stabilized with calcium alginate microspheres loaded with titanium dioxide nanoparticles (Alg@TiO2 microspheres) was designed to be used as a sunscreen component. By emulsification-gel method, the Pickering emulsion stabilized by hydrophobic TiO2 nanoparticles was used as a template, and the internal aqueous phase was gelled. The TiO2 nanoparticles were fixed on the surface of calcium alginate microspheres. The prepared microspheres were characterized by scanning electron microscopy, elemental analysis, thermogravimetric analysis and wettability. The effects of oil/water ratio and microsphere content on Pickering emulsion were investigated, and the type of emulsion was explored, and the long-term storage stability was tested. The results of SEM and elemental analysis showed that the Alg@TiO2 microspheres were spherical in shape and contained TiO2 nanoparticles on the surface, and the size of Alg@TiO2 microspheres was approximately 2-6 μm. TGA results showed that the content of TiO2 nanoparticles in Alg@TiO2 microspheres was 43%. Wettability test showed that the three-phase contact angle between the microspheres and oil and water was 120°. When the oil/water ratio was 1∶1 and the mass fraction of microspheres was 3%, stable Pickering emulsion was formed with the largest emulsion volume fraction and the smallest droplet diameter. The emulsion type was water-in-oil type (W/O type). The emulsion remained stable after 100 days at room temperature, facilitating the shelf life of the emulsion cosmetics. In UV absorption tests, the Pickering emulsion showed superior sunscreen performance compared with the other three types of sunscreens, including a commercially available sunscreen. This Pickering emulsion has been demonstrated to be easy to be cleaned as shown in skin surface cleaning experiments. The Pickering emulsion with high stability and excellent sunscreen performance as a sunscreen component is expected to promote the application of Pickering emulsions in daily chemical industry and promote the research and development of new cosmetics.

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    Lecture of science and technology
    Preparation, properties and applications of natural biomass materials (Ⅲ)Glycosaminoglycan for medical and skin care applications: hyaluronic acid
    Shi Jing,Feng Yun,Bao Jie,Fan Jianru,Xu Guiyun,Fan Jinshi
    2022, 52 (3):  237-244.  doi: 10.3969/j.issn.1001-1803.2022.03.002
    Abstract ( 407 )   HTML ( 36 )   PDF (1367KB) ( 438 )  

    Hyaluronic acid is a kind of high molecular weight glycosaminoglycan which naturally exists in a variety of living bodies. Hyaluronic acid possesses vital physiological functions, such as moisturizing, antibiosis and antiphlogosis, anti-oxidation, anti-aging, lubricating arthrosis, and regulating osmotic pressure. As a type of natural non-toxic, excellent biocompatible and degradable bioactive substance, hyaluronic acid has a unique spiral column molecular configuration, and it has many active sites (hydroxyl group, amide group and glycosidic bond) in its molecular chain, which could be modified to offer more and better functions. Up to now, hyaluronic acid and its derivatives, composites and blends have been widely used in medical treatment, cosmetics, food and other fields. In this review, the name, structure and source of hyaluronic acid, as well as its physicochemical properties, physiological functions, preparation methods and recent application progress were introduced. The development prospect and research trend of hyaluronic acid were also pointed out.

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    Development and application
    Adaptability study on a compound system for cooperative oil displacement in fractured low-permeability reservoir
    Yue Wencheng,Fan Peng,Wang Kai,Zhao Hui,Liu An,Yang Hong
    2022, 52 (3):  245-252.  doi: 10.3969/j.issn.1001-1803.2022.03.003
    Abstract ( 177 )   HTML ( 12 )   PDF (1389KB) ( 202 )  

    In the low-permeability reservoir, injection water is easy to flow along the high-permeability strips after simply profile control on the micro-fractures, which induces severe problems in the reservoir development. In this work, the foaming and stabilizing performance of a foam system and the gelling properties of a modified starch gel were evaluated. Then, the microadjustment and flooding of the foam and the collaborative oil displacement experiment of this compound system with fractured low-permeability core were carried out. The adaptability of collaborative oil displacement was verified with radial flow model, and the actual reservoir pattern was simulated. The experimental results show that the optimal mass concentrations of foaming agent and foam stabilizer are 0.5% and 0.1%, respectively. The strength and breakthrough pressure of starch gel system is high. After foam injection, the micro oil displacement efficiency of small pores during further water flooding is 14.21% higher than that of previous water flooding. And when the permeability ratio is approximately 30, its profile control performance is better. In the process of water flooding in fractured low-permeability reservoir, the collaborative oil displacement efficiency of modified starch gel combined with foam is best, which can increase the recovery by 22.17% and 46.07% as respectively compared with that of single use of modified starch gel or foam system. Moreover, the radial flow model validation experiment shows that the adaptability of this method is good in fractured low-permeability reservoir.

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    Study on preparation and performances of high suspension ability detergent
    Zhang Yun,Li Chen,Yu Sihan,Liu Dong
    2022, 52 (3):  253-257.  doi: 10.3969/j.issn.1001-1803.2022.03.004
    Abstract ( 254 )   HTML ( 20 )   PDF (1036KB) ( 228 )  

    In order to prepare detergents with high suspension ability, low viscosity, high transparency and low film-forming ability, two monomers of ethyl acrylate and methacrylic acid were used to prepare the polymer as the suspending agent in detergent (experimental group A). The influence of different monomer ratios on the suspension ability of the suspension agent was investigated. The viscosity and turbidity, suspension ability, film-forming ability and shear thinning ability in detergent of the experimental group A was compared with two commonly used acrylic suspension agents, namely Carbopol® Aqua SF-1 Polymer (control group B) and Carbopol® Aqua SF-2CN Polymer (control group C). The results show that the ductility in application of the experimental group A is the best due to the smallest viscosity in the same experimental conditions. When the mass fraction of the suspending agent is ≥1.8%, all three suspending agents have good transparency and suspending ability. The film forming ability of the experimental group A is the worst, therefore it is not easy to block the pump head. The spray extrusion strength and spray uniformity of the experimental group A are better than those of the control group B and the control group C. Overall, the performances of the experimental group A are the best.

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    Study on purification and filtration process of fatty acid methyl ester ethoxylate
    Dong Zhenpeng,Tian Wei
    2022, 52 (3):  258-262.  doi: 10.3969/j.issn.1001-1803.2022.03.005
    Abstract ( 221 )   HTML ( 18 )   PDF (1147KB) ( 152 )  

    In this paper, the filtration process of FMEE prepared by calcium catalyst was studied. The viscosity of FMEE at different temperatures and gelation phase region of FMEE were measured, and the effects of sorbent type, dosage of adsorbent, types of filter aids, amount of filter aid and number of filter paper on the filtration effect were investigated. The optimal process was confirmed by filtration time, pH after filtration, particle size distribution and calcium ion content. The results show that FMEE has gel phase, which is serious with the mass fraction of 50%±5% at 20 ℃. When the mass fraction is 80%, the viscosity of FMEE decreases with the temperature increase, and the inflection point is at 70 ℃. When the adsorbent is citric acid and the mass fraction in the solution is 0.1%, the adsorption effect is better. When diatomite is used as the filter aid and the mass fraction in the solution is 0.2%, the filtration effect is the best. When the mesh number of filter paper is 500, the primary filtration yield reaches the maximum. Under the optimized process conditions, a clear and transparent solution with calcium ion content less than 10 mg/kg can be obtained, and the turbidity of filtrate can be less than 1 NTU.

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    Study on the performance of vanadium catalyst for the oxidation of SO2 by modification of H2O2/Se
    Zhao Chengzhong,Hu Feifei,Fan Xin,Dang Wei,Lin Qian,Cao Jianxin,Pan Hongyan
    2022, 52 (3):  263-269.  doi: 10.3969/j.issn.1001-1803.2022.03.006
    Abstract ( 174 )   HTML ( 12 )   PDF (1680KB) ( 283 )  

    A new preparation method of H2O2/Se modified vanadium based catalysts was proposed in this paper. The catalysts were characterized by XRF, XRD, SEM, MIP and TG/DSC, and tested for catalytic oxidation of SO2 to SO3. And its activity was compared with that of the commercial catalysts CHP-75 and VK-38.Results show that the catalysts V-Se/SiO2 and V@x H2O2-Se/SiO2 have clear surface pores and small grain size of active components, which provide more active sites for SO2 oxidation. Meanwhile, it also has lower melting transition temperature and more forms of molten state, which is conducive to improving their low temperature activity. Among them, the catalysts V@10% H2O2-Se/SiO2 has the highest activity for SO2 oxidation due to its optimal pore structure, pore volume, active component nanoparticle size and melting transition temperature. And the catalytic activity of this catalyst is rival to the activity of VK-38 and much high than that of CHP-75. It offers a new thought and method for the design of the high efficiency vanadium catalyst.

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    Preparation and application of diatomite-based cleaner
    Zhao Zhonghua,Zhang Jian,Sheng Xueru,Li Na,Ping Qingwei
    2022, 52 (3):  270-277.  doi: 10.3969/j.issn.1001-1803.2022.03.007
    Abstract ( 200 )   HTML ( 14 )   PDF (1259KB) ( 212 )  

    With the process of global economic integration and the development of people’s high-quality life, high-efficiency, energy-saving and multi-functional washing products are attracting more and more attention. Diatomite is a kind of biogenic siliceous sedimentary rock, mainly composed of the remains of ancient diatoms. It is loose, light, porous, water-absorbent, and strong in permeability, as well as has large specific surface area and chemically stable properties. In addition, the porous properties of diatomaceous earth can achieve functions such as humidity adjustment, dye adsorption and heavy metal ion removal. The paper introduced diatomite into traditional cleaning products, and through optimizing the types and proportions of surfactants and auxiliary materials, a new type of diatomaceous earth-based cleaning agent was prepared. Its cleaning effect and prevention of mutual dyeing, label and mildew removal and other multi-functional performance were explored. It shows that the auxiliary materials of diatomite-based cleaner need to be fine-tuned according to its different uses. Diatomite-based fabric cleaner consists of 5% diatomite, 15% AEO-9, 5% 6501, 5% AEO-7, 0.3% sodium silicate, 2% palmitic acid and 3% sodium citrate. Glass bottle cleaner comprises 5% diatomite, 15% AEO-9, 5% 6501, 5% AEO-7, 3.6% sodium silicate, 1.5% sodium sulfate, 1.8% sodium gluconate, and 7.5% sodium hydroxide. The prepared product has a good cleaning effect. In terms of fabric cleaning, the clean whiteness difference of the prepared cleaning agent on carbon black, protein and sebum stained cloth is 12.3, 3, 10.2, respectively, which are better than common cleaning products on the market, and the product can realize zero inter-dyeing of the cleaned fabric. In terms of glass cleaning, the clean whiteness difference of the prepared cleaning agent to carbon black, protein cloth is 11.26 and 4.19, respectively, which are better than common cleaning products on the market. When the temperature reaches 70 ℃, the adhesive layer on the back of the label can be effectively dissociated, and the effect is uniform. So that the label can be detached as a whole, thereby reducing secondary pollution. When the amount of cleaners is 2%, the mildew removal rate on the glass reaches 100%. The addition of diatomite improves the washing effect, dye removal and mildew removal. Diatomite can be used to formulate different cleaning agents.

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    Effects of Kushui rose (Rosa setate × Rosa rugosa) essential oil on melanin synthesis in B16 cells and its mechanism
    Wu Yani,Lv Xiaofan,Wang Ying,Tang Yin
    2022, 52 (3):  278-286.  doi: 10.3969/j.issn.1001-1803.2022.03.008
    Abstract ( 367 )   HTML ( 35 )   PDF (1588KB) ( 309 )  

    The effects of Kushui rose essential oil on melanin synthesis in mouse B16 melanoma cells were investigated and its mechanism of action was explored to provide an experimental basis for the development and application of Kushui rose essential oil as a natural active substance. The volatile components of the essential oil were analyzed by gas chromatography-mass spectrometry (GC-MS). The cell model with high melanin expression induced by α-melanocyte-stimulating hormone (α-MSH) was constructed using in vitro cultured mouse B16 cells. The effects of Kushui rose essential oil on melanocyte viability were determined by CCK8 method; the changes in melanin content and tyrosinase (Tyr) activity in B16 cells were analyzed by enzyme-linked immunosorbent assay (ELISA) and dopa oxidation method, respectively; the expression of cyclic adenosine monophosphate (cAMP)-responsive element-binding protein (CRE-binding protein, CREB), p38 MAP kinase (p38 MAPK) and extracellular signal-regulated kinase (ERK) in three signaling pathways was measured. The expression of CREB, p38 MAPK, ERK and microphthalmia-associated transcription factor (MITF) in B16 cells was determined by quantitative real-time PCR (qRT-PCR) and western blotting using Kushui rose essential oil at a mass concentration of 2 g/L for 12 h, 24 h and 48 h, respectively. qRT-PCR results showed that the expression of MITF gene was significantly inhibited after 48 h treatment of B16 cells with Kushui rose essential oil. The expression of MITF gene was down-regulated by 76%, and the expression of CREB and p38 MAPK was also significantly inhibited, in which the inhibition rates reached 54% and 41%, respectively, while the expression of ERK1 and ERK2 gradually increased with time; similar results were obtained by western blot, and the trend of the expression levels of CREB and p38 MAPK was consistent with the expression level of MITF, which decreased with time, while the expression level of ERK gradually increased with time. It demonstrates that the Kushui rose essential oil reduces intracellular melanin production through three signaling pathways: cAMP/PKA, p38 MAPK and ERK/MAPK, and thus inhibit the expression of MITF.

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    Effect of inflammatory factor TNF-α on human skin cells and screening of effective extracts
    Wang Peiyu,Quan Qianghua,Wei Jing,Gao Siyu,Wang Yiming,An Quan
    2022, 52 (3):  287-293.  doi: 10.3969/j.issn.1001-1803.2022.03.009
    Abstract ( 1872 )   HTML ( 26 )   PDF (1295KB) ( 296 )  

    In order to explore the influence of inflammatory factors on human skin, inflammatory factor TNF-α was used as a stimulant to act on human skin cells. In this study, TNF-α was used as a stimulant to stimulate human skin cells. The results show that the content of senescence related secretion phenotype, IL-6 and IL-8, in the cells increases, and the cells are under the senescence state. The contents of type I collagen per protein in human skin fibroblasts, which are treated with 20, 100 and 200 ng/mL TNF-α for 24 h, are 2.740, 2.270 and 1.595 mg, respectively, lower than those in the control group; after 4 h of treatment, the contents of MMP-1 per protein are 3.10, 3.12 and 3.10 ng, respectively, higher than those in the control group. At the same time, compared with the control group, the content of intracellular reactive oxygen species is increased, and the balance of intracellular redox system is broken after the keratinocytes exposed to TNF-α. From the above experimental results, the inflammatory factor TNF-α causes the expression of collagen in skin cells abnormal, breaks the redox system, and has a certain effect on accelerating skin aging. Therefore, TNF-α can be used as a stimulant to establish a chronic inflammatory skin aging model. Follow-up experiments established a chronic inflammatory aging model through 200 ng/mL TNF-α, and investigated and compared the inhibitory effects of vitamin C, dragon’s blood extract, and Dendrobium officinale extract on it. The results show that, compared with the control group, 0.1 mg/mL vitamin C, 0.06 mg/mL dragon’s blood, and 0.5 mg/mL Dendrobium officinale extract can effectively promote the synthesis of intracellular collagen, and the contents per unit protein are 4.95, 4.84, 4.08 mg, respectively; can inhibit the expression of MMP-1, and its contents per unit protein are 1.31, 0.84, and 1.26 ng, respectively; can clear the content of reactive oxygen species in the cells and maintain the intracellular redox balance. The results show that vitamin C, as a recognized anti-aging substance, has the same anti-inflammatory aging effect; the extract of Resina draconis and Dendrobium officinale also have certain anti-inflammatory aging effect.

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    Preparation of a papain-embedding biological membrane material and its application in the skin-whitening products
    Li Ziyi,Liu Yan,Zhang Zhao,Wu Huiqin
    2022, 52 (3):  294-301.  doi: 10.3969/j.issn.1001-1803.2022.03.010
    Abstract ( 294 )   HTML ( 14 )   PDF (1400KB) ( 327 )  

    Papain is a natural sulfhydryl protease of removing aging skin and eliminating melanin, which has skin whitening and skin rejuvenation effects. This enzyme needs to be stored at appropriate temperature, humidity and pH, otherwise it will easy lose its activity during cosmetics processing because of improper operation. Compared with free enzyme, immobilized enzyme can maintain its high efficiency and specific catalytic activity. The commonly used methods of immobilization are cross-linking and embedding. Polyacrylamide (PAM) is a linear water-soluble macromolecule with good biocompatibility and harmless to skin without irritation. It is suitable for cosmetics and commonly used as cosmetics thickener. By PAM gel embedding method, a kind of papain biological membrane with good stability and high enzyme activity could be successfully synthesized. The SEM results showed that the optimal cross-linked structure of the biological membrane was obtained when the concentration and addition amount of aluminum ions was 1.2 mol/L, and 500 μL, and the reaction time was 10 h. It is found that the enzyme activity of the skin-whitening cosmetics containing this kind of biomaterial is three times higher than that of the enzyme-containing cosmetics because of the protection from PAM gel. However, the enzyme activity in the formula of cosmetics containing biological membrane was not as good as that of biological membrane, so the influencing factors of biological membrane stability need further study. It was found that small-molecule moisturizers such as glycerine, propanediol, carbamide and sorbitol did not affect the structure of the biological membrane with embedded enzyme. The sodium hyaluronate with high molecular weight could intertwine with the PAM, making the papain-embedding biological membrane wrap more tightly, resulting in a reduced contact area between the enzyme and the substrate. It was found that PAM would interact with the emulsifiers like Tween20, Tween60, Tween80, APG0814 or M68 and induce encapsulation and sedimentation, thus destroying the stable structure of the enzyme embedded in biological membrane. It is concluded that papain-embedding biological membrane is suitable for the formulation of water-based cosmetics containing small-molecule moisturizers.

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    Reviews
    Research progress on application of fiber-type clays in daily chemical industrial products
    Tang Ying,Zhang Zhaolun,Cao Lihua,Xiong Ziyi,Zhang Xi,Feng Yongjun
    2022, 52 (3):  302-308.  doi: 10.3969/j.issn.1001-1803.2022.03.011
    Abstract ( 288 )   HTML ( 14 )   PDF (1108KB) ( 222 )  

    Fiber-type clays, including sepiolite and palygorskite (also wknown as attapulgite), are a type of natural one-dimensional clay mineral with fibrous crystal structure and water-rich magnesium aluminosilicate. China has the largest mineral reserves of attapulgite in the world, about 460 million tons of proven reserves, accounting for more than 70% of the world’s total reserves. Special crystal structures (rods, fibers or fiber assemblies) and neatly arranged nano-pores endow fiber-type clays with excellent ion exchange capacity, adsorption properties, rheological regulation and carrier functions, which hold enormous potential to be exploited for application in the field of daily chemistry. In recent years, the application of fiber clay in personal care products, detergents and other daily chemical consumer products is growing rapidly. Attapulgite has been used as a natural mineral ingredient in toothpaste, facial mask, face cream, shampoo and facial cleanser for oil controlling, skin cleansing and anti-microbial functionalities. In this paper, the application characteristics and related mechanisms of fiber-type clay minerals in daily chemical industry are reviewed from the aspects of rheological modification, UV protection, coloration, bacteriostasis, anti-inflammation, controlled adsorption and release as well as the related toxicological issues. The current problems and challenges of fiber-type clays in daily chemical industry are summarized, which provide important references for Chinese researchers to make full use of this type of characteristic clay minerals and to further develop high-tech and high-value daily chemical products.

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    Application analysis of rapid microbial counting method in the detection of aerobic bacterial count in cosmetics
    Liu Feng,Wang Xiaochong,Luo Jun,Wang Xiaowei,Ying Guohong
    2022, 52 (3):  309-315.  doi: 10.3969/j.issn.1001-1803.2022.03.012
    Abstract ( 312 )   HTML ( 14 )   PDF (961KB) ( 231 )  

    The plate count method has been used as a classical method at home and abroad for the aerobic bacterial count in cosmetics, which is simple to operate, but it takes a long time to complete the entire detection process. With the development of microbiological technology, a variety of rapid microbial counting methods based on various principles have been gradually developed. By comparing the advantages and disadvantages of the plate count methods and various rapid microbial counting methods for the aerobic bacterial count in cosmetics, the length of detection time, the accuracy of the aerobic bacterial count, and the feasibility of rapid microbial counting method in the detection of aerobic bacterial count in cosmetics were comprehensively considered. It can be concluded that the fluorescence microscopy counting method and flow cytometry counting method have potential in the detection of aerobic bacterial count in cosmetics. The reasons are as follows, TEMPO® counting method, molecular biology counting method, ELISA (enzyme-linked immunosorbent assay) counting method, optical biosensors counting method, and mass spectrometry counting method have high specificity for bacteria and are only suitable for quantification of certain microorganisms, while microbial metabolism counting method, microfluidics counting methods, MicroSnapTM counting method, and SimplateTM counting method require microbial culture, thus preservatives in cosmetics will affect the accuracy of the total number of microorganisms in the sample. Although the fluorescence intensity counting method is suitable for the aerobic bacterial count in cosmetics, its sensitivity is quite low. The fluorescence microscopy counting method and flow cytometry counting method are suitable for the aerobic bacterial count in cosmetics for two reasons. The first reason is that the fluorescence microscopy counting method and flow cytometry counting method directly count the number of microorganisms in the sample so that the detection time is shorter. The second reason is that there is no need for microbial culture. Therefore, there is no need to consider the inhibitory effect of preservatives in cosmetics on microbial growth, so that the detection accuracy is higher. The introduction of rapid microbial counting methods into the standard system of the aerobic bacterial count in cosmetics, as a supplement to the current standard, is of great significance for aerobic bacterial count in cosmetics.

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    Research on daily chemical packaging design based on green and low-carbon concept
    Li Ya
    2022, 52 (3):  316-321.  doi: 10.3969/j.issn.1001-1803.2022.03.013
    Abstract ( 218 )   HTML ( 10 )   PDF (988KB) ( 450 )  

    With the rapid development of social economy in recent years, people’s quality of life is constantly improving, and the public has higher requirements for product quality. As an essential daily necessity in life, its packaging is also an important part of the product. In order to follow the country’s sustainable development strategy, promote green and low-carbon daily chemical packaging, and achieve harmony between man and nature, green and low-carbon packaging has been recognized by more and more people. It will inevitably have more room for development in the future. From the perspective of the concept of green and low-carbon, this paper analyzes the characteristics and existing problems of the country’s current daily chemical packaging, and studies the essential characteristics and structural design requirements of daily chemical packaging under the concept of green and low-carbon. The characteristics of simplicity and recyclability are described and analyzed through specific cases. Combined with the relationship between environmental protection and daily chemical packaging design, the importance of green and low-carbon design is proved by case studies. Focusing on the classification characteristics of green and low-carbon daily chemical packaging materials, the paper analyzes the development of daily chemical packaging design under the concept of green and low-carbon. Its future prospects and application value are expounded and prospected.

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    Analytical methods and testing
    Study on transdermal absorption and skin irritation of fluorescent whitening agents in facial mask
    Zhang Hongyan,Shi Xiaofeng,Wang Xiaoqiao,Liu Xingguo,Liu Yapeng,Li Yun
    2022, 52 (3):  322-327.  doi: 10.3969/j.issn.1001-1803.2022.03.014
    Abstract ( 285 )   HTML ( 14 )   PDF (1382KB) ( 214 )  

    In order to study the transdermal absorption characteristics and skin irritation of the fluorescent whitening agents (FWAs) in the facial mask, the content of 5 pyrazoline fat-soluble FWAs in the receiving solution was determined by high performance liquid chromatography triple quadrupole liquid chromatography mass spectrometry (HPLC-MS/MS) with the modified Franz transdermal diffusion cell and the abdominal skin of male rats in vitro. The cumulative penetration amount of 5 pyrazoline fat-soluble FWAs at different time points was calculated, and the FWAs remained in the skin was detected at the end of the experiment. The skin irritation test was carried out using rabbits according to the requirements of skin irritation test in “Safety and Technical Standards for Cosmetics” (2015 Edition). The results show that there is good linear relationship between the five fat-soluble FWAs determined by HPLC-MS/MS in their respective concentration ranges. The correlation coefficients (r 2) are all greater than 0.999. The detection limits are 0.5-10.0 pg and the lower limits of quantification are 2.0-30.0 pg. The average recoveries and relative standard deviations are 95.2%-102.1% and 1.8%-4.2%, respectively. The liposoluble FWAs C.I.162 in the mask could penetrate into the skin, and the transdermal diffusion within 0-36 h is in accordance with zero order kinetics equation. C.I.135, C.I.185, C.I.367 and C.I.368 are absorbed in the skin but not through the skin in a short period. Skin irritation test shows that 5 pyrazoline liposoluble FWAs in facial mask have no irritation on rabbit skin. It is suggested that the fat-soluble FWAs are easy to migrate to the stratum corneum or subcutaneous layer of the skin and have no iiritating effect on mammalian skin.

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    Determination of 39 sex hormones in oil-based cosmetics by ultra-performance liquid chromatography-tandem mass spectrometry
    Hu Bei,Li Lixia,Liu Hong,Huang Wei,Ding Xiaoping
    2022, 52 (3):  328-336.  doi: 10.3969/j.issn.1001-1803.2022.03.015
    Abstract ( 219 )   HTML ( 11 )   PDF (1094KB) ( 211 )  

    An ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed for the determination of 39 sex hormones in oil-based cosmetics. The sample was dispersed with n-hexane, then extracted with 70% acetonitrile, and separated on a CORTECS C18 (2.1 mm×150 mm, 2.7 μm) column by gradient elution using acetonitrile-water as mobile phase. The analysis was performed under multiple reaction monitoring (MRM) mode. The results showed that the matrix effects of 39 sex hormones were 0.78-1.26. The limits of detection (LODs) and limits of quantitation (LOQs) for 39 sex hormones were in the range of 0.6-2.3 μg/L and 1.9~6.8 μg/L, respectively. There was good linear relationship for 39 sex hormones in the mass concentration range of 1.87-67.41 μg/L with their correlation coefficients (r) all above 0.995. The average recoveries at three spiked levels of 0.25, 0.50 and 1.00 μg/g were in the range of 81.7%-110.6%, with relative standard deviations (RSDs, n=6) of 1.2%-14.1%. The simplicity and accuracy of this method make it suitable for the analysis of sex hormones in oil-based cosmetics.

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    Simultaneous determination of 16 preservatives, sunscreens and anti-dandruffs in cosmetics by HPLC
    Chen Yan,Bao Xijun,Yan Xiufang,Liu Jianning,Guo Fang,Niu Wenxia
    2022, 52 (3):  337-344.  doi: 10.3969/j.issn.1001-1803.2022.03.016
    Abstract ( 324 )   HTML ( 21 )   PDF (1044KB) ( 279 )  

    A method based on HPLC was established for the determination of 16 components in cosmetics including 10 types of preservatives, 4 types of sunscreens and 2 types of anti-dandruffs. The amount of 0.5 g of the cosmetic product was dissolved in methanol in a 10 mL volumetric flask and was ultrasonically extracted for 30 min. The extract was filtered through a 0.22 μm membrane, and then 10 μL solution was introduced onto an Eclipse Plus C18 column (250 mm×0.46 mm×5 μm) with methanol-0.5 mmol/L EDTA-2Na aqueous solution (pH=3.06) as mobile phase by gradient elution. The 16 components were separated at multiple wavelengths of the DAD detector. These preservatives, sunscreen agents and anti-dandruffs could be analyzed within 50 min simultaneously. The external standard method was employed for quantitative determination. The relative standard deviation of the method is 2.2%-6.5%, and the recovery is 90.9%-109.7%. The limits of detection (LODs, S/N=3) and limits of quantification (LOQs,S/N=10) of 16 components were determined. By this method, different extraction solvent, extraction time and mobile phase were compared. Among these, methanol is used as extraction solvent for 30 minutes and methanol-0.5 mmol/LEDTA-2Na aqueous solution (pH=3.06) as mobile phase shows good linear relationship in their respective mass concentration range, with the correlation coefficients higher than 0.999 0. This method has high accuracy and precision. 30 products in the market were analyzed, and the results show that phenoxyethanol, benzoic acid, and methyl 4-hydroxybenzoate are the most commonly added preservatives in cosmetics. For the four sunscreens, octyl 4-methoxycinnamate is the most frequently added. Ketoconazole is not detected in these products. In these products, all of the 16 components are lower than the relevant limits in China. This method provides technical support for market supervision and laboratory testing, which also can meet their practical testing requirements.

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