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    22 December 2021, Volume 51 Issue 12 Previous Issue    Next Issue
    Basic research
    Detection of dodecyltrimethylammonium bromide based on aggregation-induced emission phenomenon
    Sun Qing,Fang Yinjun,Liu Xuefeng
    2021, 51 (12):  1163-1170.  doi: 10.3969/j.issn.1001-1803.2021.12.001
    Abstract ( 261 )   HTML ( 85 )   PDF (1400KB) ( 232 )  

    Cationic surfactants have obvious toxicity to microorganisms in soil and water. Methods for fast and sensitive analysis and detection of cationic surfactants are important tools for monitoring the discharge of cationic surfactants. Aggregation-induced emission (AIE) phenomenon analysis is an emerging and fast method to detect surfactants. However, the analysis of cationic surfactants based on AIE phenomenon has not been reported. Therefore, a “turn-on” fluorescence method for detecting dodecyltrimethylammonium bromide (DTAB) in water was established by using a water-soluble AIE probe, 1, 1, 2, 2-tetrakis[4-(3-sulfonatopropoxyl)phenyl] ethylene salt (TSTPE), and using DTAB as the model. The results showed that free TSTPE was only weakly emissive in water; after binding with DTAB by electrostatic interaction, its fluorescence emission intensity (F) was significantly enhanced and was further increased with the increase of DTAB concentration (c). When the concentration of TSTPE was 4.5×10 -5 mol/L, the linear response range of F vs. c was around 1.05×10 -4~1.7×10-4 mol/L, and the detection limit was approximately 5.7×10-7mol/L. The fluorescence emission of TSTPE-DTAB mixed system had good stability in the pH range of 3~10; three inorganic salts, NaCl, KCl and NaNO3, had little interference with the fluorescence emission of the TSTPE-DTAB mixture, and the recovery rate of DTAB in simulated water samples was not less than 95%.

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    Lecture of science and technology
    Cosmetic emulsions and new technologies of emulsification (Ⅵ) Liquid marbles and cosmetics
    Chen Fengfeng,Gong Suijing,Chen Wenjing,Sun Yajuan,Yang Cheng,Li Yunxing
    2021, 51 (12):  1171-1178.  doi: 10.3969/j.issn.1001-1803.2021.12.002
    Abstract ( 661 )   HTML ( 30 )   PDF (1219KB) ( 454 )  

    Liquid marbles are a type of unusual soft matter that combines properties of liquid and solid by producing a lyophobic adsorbed layer of solid particles on the surface of liquid droplets. Despite the simple structure thereof, this novel soft matter has numerous unique physical and chemical properties, making it promising in a wide range of applications, particularly in cosmetics, which should be the most promising and feasible. However, there are still some disadvantages to using liquid marbles, e.g., quick evaporation of the interior droplet and uncontrollable mechanical strength of the outer shell. Herein, the preparation methods, formation mechanism and material selection have been reviewed, followed by a discussion of the physical and chemical properties of liquid marbles, with a focus on the evaporation rate of the interior droplet and the mechanical strength of the outer shell. Finally, the current state of application and the challenges of liquid marbles in cosmetics have been summarized.

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    Development and application
    Study on the preparation and performance of water and oil super-phobic coating on the surface of the turbine for monitoring the flow of heavy oil
    Song Hai,Zhang Menghua,An Peng,Wu Yuanpeng
    2021, 51 (12):  1179-1185.  doi: 10.3969/j.issn.1001-1803.2021.12.003
    Abstract ( 191 )   HTML ( 8 )   PDF (1414KB) ( 249 )  

    The water and oil super-phobic coating precursor with a micro-nano structure was produced by adding structure control agents to the substrate which was composed of the hydrolysis products of ethyl orthosilicate and fluorinated decyl trimethoxysilane, and after spraying and curing, a coating with water and oil super-phobicity could be formed. Using highly fluorinated silicon materials and surface microstructure control agents, the wettability of the solid surface has been controlled by changing the surface free energy and surface morphology. The effects of the type and content of structure control agents and the spraying conditions (spraying volume, substrate temperature, and spraying distance) on the properties of the coatings were investigated. The silica nanotubes made by ourselves with natural halloysite (nanotube), sepiolite (nanofilament) and montmorillonite (nanoflake) were selected as microstructure control fillers. The experimental results showed that the water and oil super-phobic coating with the best performance was prepared by using fibrous silica nanotubes as the microstructure control filler. By adding 5 g/L of silica nanotubes to the fluorosilicone polymer, the coating obtained could significantly increase the contact angle of heavy oil and decrease the roll angle of heavy oil. Increasing the mass concentration of silica nanotubes to 15 and 20 g/L had no significant effect on the surface microstructure and water and oil super-phobicity. During its formation, a large number of Si-Si bonds formed and the coating could be used for a long time at 160 ℃ and was not subject to salt corrosion. The optimal spraying conditions were silica nanotube mass concentration of 10 g/L, spraying volume of 10 mL, substrate temperature of 150 ℃, and spraying distance of 6 cm. The turbine coated with the water and oil super-phobic material could meet the speed measurement requirements under thick oil conditions, ensuring the normal operation of the turbine flowmeter in the monitoring and development of thick oil and solving the problem of thick oil sticking to the turbine.

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    Aqueous two-phase Pickering emulsions stabilized by the CLAA@CaCO3 nanoparticles
    Hu Jiawen,Fan Ye,Fang Yun,Wang Hong
    2021, 51 (12):  1186-1191.  doi: 10.3969/j.issn.1001-1803.2021.12.004
    Abstract ( 249 )   HTML ( 13 )   PDF (1358KB) ( 264 )  

    Aqueous two-phase system (ATPS) with the advantages of low toxicity, environmental friendliness, and good biocompatibility is often used in the field of separation and purification of biological substances. However, ATPS emulsions (the most common name is water-in-water emulsion) are much less known than oil-in-water or water-in-oil emulsions, since amphiphiles such as surfactants are difficult to adsorb on the water-water interface due to the large thickness of the water-water interface and the corresponding ultralow interfacial tension. Therefore, it is a challenge to develop effective stabilizers for water-in-water emulsions. Colloidal particles are one of the commonly used emulsifiers to stabilize water-in-water emulsion. Herein, CLAA@CaCO3 nanoparticles (NPs) were prepared via adsorbing conjugated linoleic acid admicelle (CLAA) on the surface of CaCO3 nanoparticles followed by stabilizing CLA molecules through self-crosslinking of conjugated double bonds in the CLA molecules by thermal polymerization at 80 ℃, which was confirmed by UV, FT-IR and TG analyses. The phase diagram of the ATPS composed of sodium sulfate and polyethyleneglycol 20000 (PEG 20000) was drawn and the binodal curve and tie lines were established. Subsequently, the CLAA@CaCO3 NPs were used as emulsifiers to stabilize the Pickering emulsions of Na2SO4/PEG 20000 ATPS. The results show that the CLAA@CaCO3 NPs can stabilize the PEG-in-Na2SO4 Pickering emulsions of ATPS when the mass fraction of the CLAA@CaCO3 NPs is 0.1%. Emulsions with different two-phase mass ratios on the same tie line (TL) can remain stable and the droplet size is around 50 μm. Moreover, the PEG-in-Na2SO4 Pickering emulsions with two-phase mass ratios on TL-1, TL-2 and TL-3 respectively have good long-term stability. It is found that the concentrations of the two solutes in the system should be greater than a lowest threshold concentration as indicated between TL-3 and TL-4 in order to obtain the stable Pickering emulsions of ATPS.

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    Pharmacodynamic study of an anti-photoaging composition and preparation of a gel mask
    Wu Qi,Jin Xin,Yang Xiaoqian,Zhi Hui,Wu Nan,Zhang Hui
    2021, 51 (12):  1192-1201.  doi: 10.3969/j.issn.1001-1803.2021.12.005
    Abstract ( 280 )   HTML ( 16 )   PDF (1938KB) ( 391 )  

    Ginsenosides, velvet antler peptides, sodium hyaluronate and cod collagen are used to make a composition to explore its anti-aging effect and prepare a gel mask. Through ultraviolet (UVB) induced human immortalized keratinocytes (HaCaT) and human dermal fibroblasts (HDF-α) to establish a light injury model, MTT method was used to determine the effects of different concentrations of compositions on cell viability, and enzyme-linked immunosorbent assay was used to determine the contents of superoxide dismutase (SOD), glutathione peroxidase (GSH-Px) and matrix metalloproteinase (MMP-9) in the cell supernatant. The composition was prepared into a gel mask, and the carbomer dosage, drug loading, and pH value were used as the inspection factors, and the comprehensive score of the gel mask was used as the evaluation index. The response surface method was used to screen the optimal process parameters to obtain the best preparation process for the gel mask. The test results show that compared with the blank group, the cell viability of the model group is significantly reduced (P<0.01). Compared with the model group, when the mass concentration of the composition reaches 50 μg/mL, the survival rate of HaCaT cells is 89.47%±1.81%, SOD content is (39.56±0.29) ng/mL, GSH-Px content is (41.62±0.40) ng/mL, MMP-9 content is (5.46±0.21) ng/mL. While the survival rate of HDF-α cells is 81.04%±4.09%, SOD content is (38.76±0.29) ng/mL, the content of GSH-Px is (44.28±0.05) ng/mL, and the content of MMP-9 is (4.91±0.13) ng/mL. Therefore, 50 μg/mL composition can significantly increase the activity of HaCaT cells and HDF-α cells, promote the secretion level of SOD and GSH-Px, reduce the secretion level of MMP-9, and it has a certain protective effect on HaCaT cells and HDF-α cells against light injury. Through the experimental optimization of the response surface method, the optimal process parameters of the gel mask are as follows: the dosage of carbomer is 0.6%, the drug loading is 1.3 g, and the pH=6. The gel mask prepared according to the optimal process parameters has a smooth appearance, uniformity and fineness, moderate viscosity, and good spreadability, which provides basic research for the further development of the product.

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    Antioxidant activity analysis and quality control of cosmetic ingredients from Erigeron breviscapus
    Li Qian,Xu Ming,Xiao Ruyue,Luo Chun,Li Zhanguo,Mei Shuangxi
    2021, 51 (12):  1202-1207.  doi: 10.3969/j.issn.1001-1803.2021.12.006
    Abstract ( 225 )   HTML ( 10 )   PDF (1115KB) ( 241 )  

    Erigeron breviscapus (vant.) Hand. Mazz. is one of the most important traditional Chinese medicinal plants for cardiopathy. Erigeron breviscapus mainly contains flavonoids and caffeic acids, which have obvious antioxidant activities. To study the possibility of developing Erigeron breviscapus as a cosmetics material, the antioxidant activity of Erigeron breviscapus cosmetic ingredients (EBCI) was studied and a method for simultaneous determination of two index compounds therein was established. The scavenging activities of EBCI against DPPH, ABTS and ·OH radicals were evaluated by in vitro method. The effects of EBCI on cell viability and glutathione (GSH) content were investigated by using H2O2-induced damage in HHF-1 cells. HPLC method for simultaneous determination of scutellarin and 4,5-dicaffeoylquinic acid in EBCI was established. The results show that EBCI have scavenging activities against DPPH, ABTS and ·OH radicals, with IC50 values being 46.93, 91.36 and 89.37 μg/mL, respectively. The cell viability of H2O2-induced injury in HFF-1 cells and the GSH content in the cells could be significantly increased at the concentrations of 4 and 20 μg/mL. 4,5-Dicaffeoylquinic acid and scutellarin showed good linearity in the linear ranges of 0.008 5-0.340 9 mg/mL and 0.009 3-0.372 2 mg/mL, respectively. Average recoveries of scutellarin and 4,5-dicaffeoylquinic acid were 103.47% and 103.38% (RSD<2%), respectively. This method is accurate, simple and well reproducible, and can be used for the quality control of EBCI. It shows the antioxidant activity of EBCI in this study.

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    Study on the effects of Phyllanthus emblica extract on anti-aging and hair growth promotion
    Wu Qi,Wang Xiaoqing,Cui Ting,Zhang Zhang,Wang Fenglou,Ma Gang
    2021, 51 (12):  1208-1214.  doi: 10.3969/j.issn.1001-1803.2021.12.007
    Abstract ( 896 )   HTML ( 71 )   PDF (1537KB) ( 511 )  

    Herbal extracts which are safer and more acceptable compared with chemical compounds and hormone products, may contain agonists in the Nrf-2/HO-1 pathway that mobilize the body to produce effective endogenous antioxidant capacity delaying aging and reducing elastase content to keep skin elastic and firm. Antioxidant capacity and elastase inhibition rate of P. emblica extract were tested to obtain its effects on anti-aging. Under the action of 5α-reductase, testosterone is reduced to DHT, whereas high content of DHT is the primary cause of the AGA. Inhibiting 5α-reductase by plant extracts to reduce DHT content is an effective way to alleviate AGA. DP is the signal center of hair growth and the target of testosterone in the hair follicle which expresses rich 5α-reductase. In vitro 3D cultivation of HFDPC, an ideal detection model, can not only agglomerate them into balls to resemble growth environment in vivo, but also maintain hair induction ability. The 5α-reductase inhibiting ability, the cell viability of HFDPC after 3D cultivation and in vitro human hair growth rate were examined to acquire its effects on hair growth promotion. The results suggest that P. emblica extract is supposed to delay senescence through inhibition of oxidization and elastase activity, and to facilitate hair growth through inhibition of 5α-reductase and β-galactosidase, enhancement of HFDPC proliferation and inductivity, and promotion of in vitro human hair follicle growth. We evaluate the anti-aging and hair growth promotion effect of the P. emblica to provide reference for further researches.

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    Preparation and efficacy evaluation of mosquito repellent gel
    Zhao Mengtian,Yang Yi,Xu Jian,Jin Jiahua,Ding Liqin,Cao Gao
    2021, 51 (12):  1215-1220.  doi: 10.3969/j.issn.1001-1803.2021.12.008
    Abstract ( 573 )   HTML ( 16 )   PDF (1278KB) ( 281 )  

    We aimed to prepare a mosquito repellent gel with suitable consistency, refreshing skin feeling, safe and convenient use and long effective mosquito repellent time. In this paper, the effects of the mixture of different solubilizers, the dosage of different thickeners and the types and dosage of repellent on mosquito repellent gel were studied. The stability, appearance and skin sensation of mosquito repellent gel were evaluated by the combination of physical and chemical indexes such as cold and heat resistance and sensation, so as to determine the better basic formula. The mosquito repellent efficacy and safety of the better basic formula were evaluated. Then, in order to meet the needs of different target users, plant extracts with antibacterial and antioxidant activities were added to the basic gel formulation, and its effect on gel stability was observed. The results show that the gel prepared by the combination of 30% PEG400 and 15% propylene glycol can not only effectively increase the solubility of the repellent in water, but also has good stability and refreshing skin feeling. 0.8% carbomer 940 is used as the thickening agent of the mosquito repellent gel, which has good thickening performance and can achieve ideal skin feeling. The effective mosquito repellent time of DEET, BAAPE and Ecaritin repellent gel with 7.5% repellent addition is 6.8, 8.0 and 9.3 h, respectively, and the effect of the three self-made mosquito repellent gels is better than that of the mosquito repellent toilet water containing 12.5% mosquito repellent ester on the market. The animal skin irritation and eye irritation experiments show that the prepared mosquito repellent gel has no obvious irritation to the skin, but has slight irritation to the eyes. When the plant extract with antibacterial and antioxidant efficacy is added to the basic formula of the mosquito repellent gel, the transparency of the mosquito repellent gel decreases, especially with mosquito repellent ester as repellent. The physical and chemical properties of the mosquito repellent gel were tested, and the results show that all the indexes of the mosquito repellent gel meet the relevant requirements. The performance is relatively stable, and it is expected to have a good application prospect.

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    Study on soothing and repair effects of “Franicshield” on sensitive skin
    Chen Qingsheng,Meng Xiao,Liu Ting,Li Chuzhong,Zhou Zhaofang,Gong Shengzhao
    2021, 51 (12):  1221-1227.  doi: 10.3969/j.issn.1001-1803.2021.12.009
    Abstract ( 471 )   HTML ( 30 )   PDF (1043KB) ( 485 )  

    The soothing and repair functions of “Franicshield” on sensitive skin were studied. The anti-allergy &repair composition “Franicshield” was composed of ceramide, squalane and other skin lipid components to repair the skin barrier function; sodium hyaluronate and aloe leaf water were used to replenish water and moisturize the skin; natural active extracts such as Centella asiatica, Polygonum hydropiper and Inonotus obliquus were used to reduce skin inflammation and soothe skin. The anti-inflammatory effect and eye irritation were evaluated by TNF-a release induced by LPS from mouse macrophages (RAW264.7) and erythrocyte hemolysis test. Human clinical test was used for evaluation based on three dimensions: researcher evaluation, instrument measurement and subject self-assessment. The results showed that it had no significant effect on the activity of RAW264.7 mouse macrophages, and significantly inhibited the production of TNF-a inflammatory factor induced by LPS when the mass fraction of “Franicshield” was within 20%. The erythrocyte hemolysis test showed no irritation. After using “Franicshield” for 4 weeks, the subjects’ skin erythema, scaling, smoothness and roughness were improved, and the difference was statistically significant (P<0.05). The water content of stratum corneum, TEWL value, red area change, lactic acid irritation and the relief rate of skin problems such as tingling, itching, tension and burning before and after use showed that “Franicshield” had good soothing and repair functions, and the difference was statistically significant (P<0.05). No adverse skin reactions occurred during the 4-week test, indicating that it had good safety and was suitable for people with sensitive skin.

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    Study on the performance of facial cleansers based on the mixture of a soap and an amino acid surfactant
    He Guangwen,Yan Shaowei,Zeng Yifan,Yan Jialei,Qian Jingru,Wang Jing
    2021, 51 (12):  1228-1234.  doi: 10.3969/j.issn.1001-1803.2021.12.010
    Abstract ( 791 )   HTML ( 38 )   PDF (1421KB) ( 575 )  

    According to the demand for development of facial cleansers, the suitable soap based surfactant and the amino acid surfactant were selected to prepare facial cleansers based on pure soap, pure amino acid surfactant and the mixture of soap and amino acid surfactant. The moisturizing, sebum control and mildness of the three kinds of facial cleansers were compared by volunteer evaluation, skin dyeing residue test and skin natural moisturizing factor/lipid extraction tests. The results showed that the ability of moisturizing of soap-amino acid surfactant based cleanser was higher than that of pure-soap based cleanser, and its sebum controlling property was better than that of pure-amino-acid-surfactant based cleanser. Moreover, the soap-amino acid surfactant based cleanser was the favourite one according to the volunteer evaluation. In addition, the residue of soap-amino acid surfactant based cleanser on the skin was less than that of pure-amino-acid-surfactant based cleanser, and its skin mildness was much better than that of pure-soap based cleanser. In general, the soap-amino acid surfactant based cleanser developed in this study achieves a better balance among cleansing ability, mildness and skin feeling.

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    Reviews
    Research progress on toxicology and risk assessment of zinc pyrithione as cosmetics ingredient
    Huang Xianglu,Lu Jiacan,Xing Shuxia,Sun Lei
    2021, 51 (12):  1235-1241.  doi: 10.3969/j.issn.1001-1803.2021.12.011
    Abstract ( 731 )   HTML ( 16 )   PDF (1067KB) ( 408 )  

    Zinc pyrithione (ZPT) is a commonly used anti-dandruff ingredient in cosmetics, which have attracted great attention in the cosmetic industry because of the ban on ZPT in the EU. It could be demonstrated that the acute as well as the sub-chronic toxicity of both ZPT alone or incorporated in market formulation is moderate to low in animal experiments or after practical application to humans. ZPT is-at least-a mild skin irritant but a severe eye irritant and corrosive. ZPT is considered not to be a skin sensitizer based on guinea pig studies. Concerning human data, ZPT (or PT moiety part) has a low potential to induce contact hypersensitivity when tested per se or as part of a cosmetic formulation. ZPT is rapidly and extensively absorbed after oral dosing, is distributed throughout the body, and is not concentrated in any particular tissue. The primary route of excretion of ZPT is via the urine. In a combined chronic toxicity/carcinogenicity study, the dose of 0.5 mg/kg bw/d is considered as NOAEL by the SCCS. It considers ZPT as a non-genotoxic and non-mutagenic compound in vivo. From the studies performed by the oral or dermal route with ZPT, there is no evidence of carcinogenic potential up to dermal doses of 100 mg/kg bw/d and up to oral doses of 2.5 mg/kg bw/d.It is not indicated any potential concern to humans regarding adverse effects on fertility but on development which is most likely attributable to maternal toxicity. It is under a significant adverse impact on the aquatic ecological environment. The SCCS considers ZPT as safe when used as an anti-dandruff in rinse-off hair products up to a maximum content of 1%, while the preliminary evaluation of the research group believes that the maximum content of 1.5% in hair products in China as an anti-dandruff agent is safe. In view of the impact of the EU ZPT ban on China’s cosmetics industry, it is suggested to continuously track the legislative formulation and safety of ZPT in cosmetics and to make good technical reserves, so as to provide reference for perfecting the supervision system of cosmetics in China. Meanwhile, multi-channel risk communication should be made to guide the improvement of the product formula, and the setting of product transition period should be comprehensively considered. The industry should be encouraged to carry out research and development of new cosmetic ingredients and increase the variety of optional cosmetics ingredients to promote the healthy development of the cosmetics industry.

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    Analysis about whether microorganisms that can effectively degrade fluorocarbon chains would appear in the natural environment
    Xiao Zibing,Xing Hang,Dou Zengpei,Xiao Jinxin
    2021, 51 (12):  1242-1249.  doi: 10.3969/j.issn.1001-1803.2021.12.012
    Abstract ( 304 )   HTML ( 8 )   PDF (1161KB) ( 337 )  

    The fluorocarbon chains of PFAS (per- and polyfluoroalkylated substances) are highly chemically inert. With the increasing awareness of protection of environment and health, the extensive use of PFAS has aroused public concern. PFAS are irreplaceable in many application fields, especially in the cases of high-tech applications or harsh conditions. Therefore, the most active coping strategy should be to explore feasible treatment methods. Compared with physical or chemical treatment, biodegradation is advantageous in convenient applied conditions and being energy-saving and cost-effective. However, up to now, no microorganisms have been found to be qualified to “effectively” degrade PFAS, i.e., to completely break down PFAS in a satisfactory range of time by destroying the C-F bonds. It means that a desired species of microorganisms must meet the dual requirements of degradation degree and degradation efficiency. Herein, we have discussed whether microorganisms, that can effectively break down the fluorocarbon chain, could appear in the natural environment, as well as the strategies that can be adopted to simulate this process in laboratory. Some evidence of the microbial degradation of PFAS has also been listed. In the future, it is expected that human beings can develop and cultivate microbial species that can effectively break down fluorocarbon chains.

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    Analytical methods and testing
    Determination of 23 illegally added antibiotics by UPLC-ESI-Q-TOF/MS in cosmetics
    Zheng Jiaxin,Jia Changping
    2021, 51 (12):  1250-1258.  doi: 10.3969/j.issn.1001-1803.2021.12.013
    Abstract ( 238 )   HTML ( 7 )   PDF (1304KB) ( 253 )  

    The aim of the study is to develop an ultra high performance liquid chromatography-tandem mass spectrometry method for the identification and determination of 23 antibiotics in cosmetics. The samples were extracted by ultrasonic machine with acetonitrile, and the separation was executed on a column using a mobile phase consisting of 0.1% formic acid (A), and 0.1% formic acid- acetonitrile (B). The mass spectrometer was operated in positive ion mode, the determination was conducted in MS scan mode by the external standard method, and confirmatory analysis for target compounds was performed with the retention time and MS2 scan. The result show that the linear relationship of the 23 antibiotics in the linear range is good, and the correlation coefficient is greater than 0.995. The detection limit are between 0.05-1.36 μg/g, and the average recovery rate is in the range of 74.1%-125.5%, with RSD within 2.3%-13.2%. One batch of positive sample is detected in 22 batches of the samples. Trimethoprim is detected in cosmetics for the first time. The established method is simple, selective, sensitive and accurate, and can be used for determination of antibiotics in cosmetics.

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    Simultaneous determination of 63 hormone drugs in facial masks by UHPLC-MS/MS
    Qiao Yasen,Dong Yalei,Huang Chuanfeng,Wang Haiyan,Sun Lei
    2021, 51 (12):  1259-1268.  doi: 10.3969/j.issn.1001-1803.2021.12.014
    Abstract ( 513 )   HTML ( 16 )   PDF (1152KB) ( 299 )  

    An UHPLC-MS/MS method for the determination of 63 hormone drugs in facial mask cosmetics was established. The pretreatment conditions and mass spectrometry parameters were optimized. The samples were extracted with acetonitrile by ultrasonic-assisted liquid-liquid extraction. Acetonitrile and water were employed as mobile phases and gradient elution was performed. The UHPLC separation was carried out on a Shim-pack XR-ODSⅢ column (2.0 mm×150 mm). The samples were detected by tandem mass spectrometry detector with scheduled multiple reaction monitoring (Scheduled MRM) scanning method. And 63 kinds of glucocorticoids and sex hormones were scanned through simultaneous collection of positive and negative ions. Quantitative analysis was carried out by matrix standard curve with the peak areas of the daughter ions on high intensity. The detection limit, quantitative limit and linear equation of 63 hormone drugs were confirmed. The average recoveries are 71.5%-119.5%, and the RSD are less than 19.2%, indicating good recovery and high precision. This method is simple, sensitive and accurate, which can be employed to simultaneously detect illegal addition of hormone drugs in facial mask cosmetics. It is suitable for high through-put detection of prohibited substances in cosmetics. This research work provides technical support for the safety and quality supervision of facial mask cosmetics.

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    Determination of 32 kinds of component in hair dyes by HPLC-MS/MS and stability analysis of dye intermediates
    Li Ruoqi,Wu Yue,Sun Ying,Li Guangning
    2021, 51 (12):  1269-1277.  doi: 10.3969/j.issn.1001-1803.2021.12.015
    Abstract ( 237 )   HTML ( 15 )   PDF (1320KB) ( 205 )  

    A method was developed for the determination of 32 kinds of component in hair dyes using high performance liquid chromatography-tandem mass spectrometry, and the stability analysis of dye intermediates. The samples were extracted with mixed solution with methyl alcohol and 2 g/L sodium bisulfite aqueous solution (V/V=2∶8). The analytes were separated on a Atlantis T3 column with 10 mmol/L ammonium formate aqueous solution (pH=8) and mixed solution with methyl alcohol and acetonitrile (V/V=1∶1) as mobile phases, and finally analyzed using electrospray ionization in positive and negative ion mode (ESI+, ESI-) with multilpe reaction monitoring (MRM). The linear ranges of the 32 dyes are from 0.005-50 mg/kg with correlation coefficients (r) more than 0.995. The matrix effects range from 4.1% to 44.6% in samples. The average recoveries are 80.2%-109.6% at the spiked levels of 0.2, 2 and 10 mg/kg. The average relative standard deviations is 0.8%-9.8% at the spiked levels of 0.5, 2 and 5 mg/kg. The limits of detection and the limits of quantification are 0.005 2-2.4 mg/kg and 0.018-7.9 mg/kg for the 32 dyes. The peak area of dyes increases by an average of 30.3% at 10 h in positive ion detection mode. The peak area of dyes decreases by an average of 29.6% at 20 h in negative ion detection mode. The method is simple, rapid and sensitive, and can provide technical support for dye detection in hair dyes. The instability of dyes can provide theoretical basis for quantitative analysis and quality control. The instability of dye intermediates can provide theoretical basis for quantitative analysis.

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    Determination of four characteristic components in Glycyrrhiza uralensis based cosmetics by LC-MS method
    Deng Yingming,Chen Yuan,Deng Meiling,Song Zengxuan
    2021, 51 (12):  1278-1282.  doi: 10.3969/j.issn.1001-1803.2021.12.016
    Abstract ( 242 )   HTML ( 15 )   PDF (1208KB) ( 337 )  

    A LC-MS method was established for determination of botanical cosmetics claimed to contain ingredients from Glycyrrhiza uralensis. The sample was dispersed by saturated solution of sodium chloride and was ultrasonically extracted with acetonitrile. 0.1% formic acid water-acetonitrile was used as the mobile phase for gradient elution at a flow rate of 0.4 mL/min. Multiple reaction monitoring (MRM) mode was used for detection. The four components had good linear relationship within their respective range. The average recovery rate was 85%-104%, the RSD was 1.1%-10.0%, and the detection limit of the method was between 1 and 15 ng/g; 12 batches of samples were tested and the coincidence rate thereof was 41.6%. The test results indicate that the presence and the amount of ingredients from Glycyrrhiza uralensis are actually relatively low in as-claimed cosmetics. In other words, there are conceptual marketing and false publicity and thus relevant supervision should be strengthened.

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