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Table of Content

    22 March 2024, Volume 54 Issue 3 Previous Issue    Next Issue
    Basic research
    Preparation and performance of betaine/AOS/Gemini ternary surfactant foam for gas well deliquification
    Zhisheng Zhang, Chanliang Shen, Jianxun Li, Yanqiang Liu, Weiwei Han, Sanbao Dong
    2024, 54 (3):  239-249.  doi: 10.3969/j.issn.2097-2806.2024.03.001
    Abstract ( 196 )   HTML ( 24 )   PDF (2759KB) ( 91 )  

    Foam-based deliquification is important to ensure the production of gas wells, therefore, there is no doubt that the development of high-performance foaming agents is extremely critical for the gas wells with high salinity, high condensate oil content and high temperature. For this reason, a highly efficient and environmentally friendly ternary foaming mixture was prepared by coconut oil amide propyl hydroxy sulfobetaine (CHSB), sodium α-olefin sulfonate (AOS) and synthetic Gemini cationic surfactant (CAGB) in this study. The results showed that the AOS/CAGB/CHSB mixture had the best performance when the molar ratio was 12∶3∶35 at the total amount of 20 mmol/L. The foam volume and half-life reached 360 mL and 30.27 min, respectively. In the foaming agent solution containing 30% methanol, the measured liquid unloading efficiency was 31%, and the foaming efficiency was 95%. With 0%-50% condensate oil, the ternary foaming mixture showed good performance. With 20% condensate oil, the liquid unloading efficiency was up to 38% and the foaming efficiency was 95%. The optimized AOS/CAGB/CHSB exhibited poor tolerance to salt ions. However, with trisodium aminotriacetate (NTA), the ternary complex system was still effective at a salinity of 150 g/L. At temperatures higher than 50 ℃, the liquid unloading efficiency of the foam also gradually increased, and the liquid unloading efficiency was above 95% at 90 ℃. In addition, the surface tension test and foam microstructure observation also confirmed the presence of synergy in foaming, foam stabilization and foam liquid unloading.

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    Performance evaluation of a system of imbibition oil displacement agent in shale reservoir
    Guofeng Li, Kainan Liu, Wenlong Mo, Teng Ma
    2024, 54 (3):  250-258.  doi: 10.3969/j.issn.2097-2806.2024.03.002
    Abstract ( 92 )   HTML ( 12 )   PDF (2881KB) ( 75 )  

    The recovery of crude oil from shale oil reservoirs remains a significant challenge due to the ultra-low permeability and complex pore structures. Surfactants have been increasingly investigated as a potential method to enhance oil recovery in unconventional reservoirs by reducing interfacial tension and altering wettability. In this work, the performance of surfactants for potential application in shale oil reservoirs was evaluated by investigating spontaneous imbibition behavior. The results showed that the interfacial tension of 0.15 wt% CA-90+0.15 wt% SDS was reduced to 1.03×10-2 mN/m under formation conditions. The wetting contact angle of the oil-wet core sheet was reduced from 135.5° to 49.5°, i.e., the wettability of the rock was changed from oil-wet to water-wet, and the capillary force was thus changed from resistance for oil imbibition to driving force. When the water content was 70%, the viscosity of the emulsion decreased to 23.4 mPa·s which was close to the viscosity of crude oil, but the fluidity was higher, which was more conducive to improving oil recovery. The dynamic adsorption capacities of 0.15 wt% CA-90 and 0.15 wt% SDS were 0.85 mg/g and 0.97 mg/g, respectively, which had good anti-adsorption ability, and the damage rate of shale permeability was less than 8%. The imbibition recovery of slick water+compounded system could reach 31.27%, which was much higher than that of spontaneous imbibition recovery in slick water system (19.43%), and the imbibition oil displacement efficiency was thus increased by 60.94%, which greatly improved the oil recovery for shale reservoirs.

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    Lecture of science and technology
    Botanical cosmetic ingredients (VII)Research and development of plant antifungal
    Jingxuan Liu, Jianming Jin, Hua Wu
    2024, 54 (3):  259-266.  doi: 10.3969/j.issn.2097-2806.2024.03.003
    Abstract ( 141 )   HTML ( 15 )   PDF (1458KB) ( 1223 )  

    This paper describes skin fungi and fungal skin infections, and summarizes the antifungal mechanism and the corresponding drug targets of the bioactive compounds from plants. The active antifungal compounds from plants include polyphenols, alkaloids, flavonoids, terpenoids, steroids and essential oils, etc. The main antifungal mechanism is inhibition of fungal cell wall and cell membrane biosynthesis. The target of cell wall biosynthesis inhibition is via inhibiting the activities of β-glucan synthetase, chitin synthase and mannan synthase. And the target of cell membrane biosynthesis inhibition is via inhibiting the synthesis of the structural components, ergosterol and sphingolipids. By inhibiting ergosterol synthetase, serine palmitoyltransferase, ceramide synthase and myo-inositol phosphatidyl ceramide synthase, the active components from plants can also directly bind to ergosterol and sphingolipids and destruct the cell membrane. In addition, phenols, alkaloids, flavonoids, terpenoids and essential oils also target mitochondrion to display antifungal activity, by inducing reactive oxygen species (ROS) accumulation, inhibiting ATP biosynthesis and proton pumps, and disrupt the mitochondrial respiration and metabolic system. This paper has reviewed the antifungal mechanisms of bioactive compounds from plants, hoping to provide a reference for the applications of plant materials in cosmetics, for a better maintaining of skin health.

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    Development and application
    Evaluation of decontamination effect of a laundry detergent for radioactive contaminants
    Zhiting Gao, Lixiao Guo, Cuidonghui Chen, Yuhang Zhang, Dan Luo, Mingliang Wu, Xiumei Tai
    2024, 54 (3):  267-272.  doi: 10.3969/j.issn.2097-2806.2024.03.004
    Abstract ( 53 )   HTML ( 8 )   PDF (2149KB) ( 29 )  

    Decontamination of the radioactively contaminated daily clothing in nuclear industry can minimize waste, reuse resources, and reduce the radiation damage to human health. Normal commercial laundry detergents can meet the requirements for removing oil and sweat stains, but they are difficult to remove radioactive nuclides such as strontium and uranium. Currently, many foreign companies have specialized products for radioactively contaminated clothing, such as HAKA and FEVDI, but there are few in China. To solve this problem, in this work, a detergent was prepared using a self-made formula. The evaluation method on decontamination effect was established with reference to GB/T 13174 and GB/T 14057.2, and the decontamination performance of the detergent was evaluated. The homemade detergent was compared with commercially available laundry detergents. The results showed that the detergent had good decontamination effects on radioactive pollutants, reaching over 80%, and its comprehensive decontamination performance was superior to commercial laundry detergents. It had good detergency for simulated stains of oil, dust and sebum. But it had poor detergency for protein stains. This detergent could meet the requirements in daily operations of nuclear industry for decontamination of radioactive contaminants, sweat stains of workers, and oil stains of machinery and equipment, which was expected to become a new product for removing radioactive contamination from daily clothing in nuclear industry.

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    Preparation and adsorption properties of porous boron nitride materials
    Yuting Duan, Yingmiao Zhao, Sui Shen, Zhenxi Lu, Bing Liang, Jiapeng Long
    2024, 54 (3):  273-281.  doi: 10.3969/j.issn.2097-2806.2024.03.005
    Abstract ( 67 )   HTML ( 3 )   PDF (1946KB) ( 37 )  

    By using the precursor conversion method, one-dimensional boron nitride fibers, two-dimensional boron nitride films and coatings, and three-dimensional boron nitride composite materials have been prepared, which cannot be prepared by traditional preparation methods. Dimethylamine, boron trichloride, ammonia and methylamine were used as raw materials to obtain the boron nitride precursor tri(methylamino) borazine by multi-step reaction, and the boron nitride porous materials were obtained by high temperature sintering. The structures of the intermediates dichlorodimethylamino borane and tri(dimethylamine) borazine and the precursor tri(methylamino) borazine were characterized by FTIR and NMR. The porous boron nitride structures and morphologies were characterized by XRD and SEM. The results show that tri(methylamino) borazine with low carbon content can be synthesized through the synthesis of precursor intermediates. The adsorption capacity of porous boron nitride materials for various metal ions was determined by investigating the adsorption capacity of porous boron nitride materials for metal ions. The results show that the porous boron nitride prepared by using precursor intermediates has high specific surface area and excellent adsorption performance, which can effectively remove the metal ions from the solution and provide new ideas for the preparation of boron nitride adsorption materials. This method solves the problems of low industrialization yield and high difficulty. The use of organic precursor method to prepare boron nitride compensates for the shortcomings of uneven element distribution, easy moisture absorption, and easy pulverization in inorganic preparation, providing new ideas for the preparation of adsorbents.

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    Efficacies and mechanisms of a formula of Chinese medicinal plants (MHC-20) against Streptococcus pyogenes
    Cuicui Hu, Daihong Zhou, Xinwan Chen, Jialing Zhong, Canquan Mao
    2024, 54 (3):  282-289.  doi: 10.3969/j.issn.2097-2806.2024.03.006
    Abstract ( 69 )   HTML ( 4 )   PDF (1938KB) ( 54 )  

    The antimicrobial properties and mechanisms of a formula of Chinese medicinal plants (MHC-20) against Streptococcus pyogenes were studied. The MIC of MHC-20 against S. pyogenes was 31.25 μg/mL or 0.31% as measured by broth micro-or macro-dilution. MHC-20 was also found to have strong killing effects on Staphylococcus aureus, Escherichia coli and Candida albicans. The results of instantaneous bactericidal activity showed that MHC-20 was able to kill S. pyogenes completely in 5 min. It could also significantly reduce the cell surface hydrophobicity and inhibit the formation of biofilm. Cell membrane permeability test showed that MHC-20 could induce the increase of relative conductivity and alkaline phosphatase, as well as the protein leakage, in a concentration-dependent manner. The results of scanning electron microscopy further confirmed that MHC-20 had a strong destructive effect on cell morphology. Finally, a mouse model of cutaneous infection with S. pyogenes was established. It was shown that MHC-20 could promote wound healing and significantly inhibit the loading concentration of S. pyogenesP<0.01); 5% MHC-20 and 20% MHC-20 significantly decreased the expression of IL-6 in serum and tissue of the mice (P<0.001). 20% MHC-20 significantly decreased the expression of leukocytes (P<0.01). In conclusion, MHC-20 had the potential to be developed into a broad-spectrum antibiotic and an effective drug for cutaneous infection with S. pyogenes.

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    Preparation and adsorption performance of tannin cured with triethylenetetramine
    Shaodi Jin, Xueer Xu, Dongya Gu
    2024, 54 (3):  290-297.  doi: 10.3969/j.issn.2097-2806.2024.03.007
    Abstract ( 57 )   HTML ( 4 )   PDF (2504KB) ( 42 )  

    An amine-modified tannin adsorbent (TETA-TA) was prepared by Mannich reaction, in which triethylenetetramine (TETA) was used to cure tannin, and its preparation process was optimized by orthogonal experiment. The structure of TETA-TA was characterized by FT-IR, SEM and BET, and the adsorption properties of the adsorbent to Cd2+ and Pb2+ were investigated at different pH, different adsorption time and different initial concentrations of metal ions. The results of orthogonal experiment showed that, when the molar ratio of tannin to TETA to formaldehyde was 1∶2∶2.5, the reaction temperature was 80 ℃, the reaction time was 4 h and the dosage of acetic acid was 4%, the experiment had the best preparation conditions. The results of adsorption indicated that, the adsorption capacity for Cd2+ and Pb2+ greatly depended on the pH, and the optimal pH values for Cd2+ and Pb2+ were both 5.0. The adsorption of Cd2+ was rapid, which could quickly reach adsorption equilibrium within 60 min, but the adsorption of Pb2+ could continue for 24 h. The adsorption process of Cd2+ and Pb2+ by TETA-TA conformed to the pseudo-second-order kinetic model, which was a chemical adsorption process. Higher initial concentrations of metal ions could lead to higher equilibrium adsorption capacity. The adsorption isotherm of Cd2+ could be well described by Langmuir equation (R2=0.995), and the theoretical maximum adsorption capacity was 150.41 mg/g. The adsorption isotherm of Pb2+ could be well fitted with Sips equation, and the theoretical maximum adsorption capacity was 210.45 mg/g. The main adsorption mechanism for Pb2+was speculated to be chelation and redox reaction between Pb2+ and hydroxyl/amine groups on the surface of the adsorbent, which were accompanied with ion exchange and electrostatic adsorption. It was also found that when more than one kind of metal ions coexisted in aqueous solution, the equilibrium adsorption capacity for each was not affected by others, implying that the TETA-TA adsorbent was effective in simultaneous removal of these ions. The test results of regeneration and reusability indicated that the TETA-TA adsorbent was suitable for repeated use for more than five times.

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    Preparation and paramagnetic study of Fe3O4-based core-shell nanostructured materials
    Keyun Hu
    2024, 54 (3):  298-304.  doi: 10.3969/j.issn.2097-2806.2024.03.008
    Abstract ( 213 )   HTML ( 2 )   PDF (2013KB) ( 66 )  

    Fe3O4@SiO2 core-shell nanostructured materials were prepared with Fe3O4 as magnetic core and SiO2 as shell. Surface hydrophilic modification of Fe3O4@SiO2 was carried out with triethoxysilane. The effects of hydrophilic modification on its paramagnetism and catalytic properties were studied. The results showed that Fe3O4 with cubic structure was the main crystal phase in the core-shell materials. The SiO2 at surface was amorphous, and the crystal structure of Fe3O4@SiO2 remained unchanged after surface hydrophilic modification. The Fe3O4@SiO2 material was irregular particles of 80-110 nm, in which the Fe3O4 was coated with SiO2. The saturated magnetization of the Fe3O4@SiO2 after hydrophilic treatment was reduced to 20.31 emu/g, indicative of superparamagnetism. This nanomaterial was applied to the wastewater containing Cd2+ for adsorption and degradation, where the removal rate was increased to 94.2%. The second-order kinetic model was more suitable for the adsorption of Cd2+ with Fe3O4@SiO2, and the correlation coefficient of the model was 0.994 3, showing good fitting. The results showed that the adsorption rate of Cd2+ by Fe3O4@SiO2 was greatly affected by chemisorption.

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    Analysis of the mechanism of anti-sensitive skin effect of cosmetic raw material Stephania tetrandra based on network pharmacology
    Wu Bi, Xiaohong Pan, Xiaoqin Tu, Shuai Yin, Hui Sun
    2024, 54 (3):  305-312.  doi: 10.3969/j.issn.2097-2806.2024.03.009
    Abstract ( 109 )   HTML ( 12 )   PDF (2549KB) ( 64 )  

    Explore the mechanism of anti-sensitive skin effect of cosmetic raw material Stephania tetrandra on sensitive skin using a network pharmacological approach. The main chemical components of Stephania tetrandra were collected through TCMSP, CNKI, PubMed and other databases, and their targets were predicted using Swiss Target Prediction, intersected with the disease targets obtained from Genecards database and then used String database to construct protein interaction (PPI) network. Cytoscape3.9.1 software was used to analyze the core targets, and the DAVID online database was used to perform GO functional analysis and KEGG pathway enrichment analysis on the core targets. The results of GO enrichment analysis show that the 39 core targets are mainly involved in various biological processes such as protein phosphorylation, signal transduction, transcriptional regulation and gene expression. The results of KEGG pathway enrichment analysis show that the anti-sensitive skin effect of Stephania tetrandra may be closely related to VEGF signaling pathway, HIF-1 signaling pathway, ErbB signaling pathway and PI3K-Akt signaling pathway. The active ingredients in Stephania tetrandra, such as Dicentrined, Cepharanthine and Fangchinoline, may exert their anti-sensitive skin effects by acting on the targets of JAK2, JAK3 and SYC, reflecting the multicomponent-multitarget-multipathway action characteristics of Stephania tetrandra.

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    Study on the anti-aging and antioxidant effects of isosinensetin
    Yaoyao Li
    2024, 54 (3):  313-319.  doi: 10.3969/j.issn.2097-2806.2024.03.010
    Abstract ( 133 )   HTML ( 17 )   PDF (1770KB) ( 78 )  

    The study aimed to investigate the anti-aging and antioxidant effects of isosinensetin (ISO) on skin aging mice induced by D-galactose (D-gal). The mice were divided into 6 groups (n=12): C group, D-gal group, D-gal+L-ISO group, D-gal+M-ISO group, D-gal+H-ISO group and D-gal+H-ISO+ML385 group. The skin aging mouse model was established by subcutaneous injection of D-gal of 1 g/ (kg·d) into the back of mice for 6 weeks. From the day of D-gal injection, mice in C group and D-gal group were applied with snow cream on their back depilation area, while mice in D-gal+L-ISO group, D-gal+M-ISO group and D-gal+H-ISO group were applied with 50, 100 and 200 mg/kg isosinensetin cream, respectively. The mice in D-gal+H-ISO+ML385 group were applied with 200 mg/kg isosinensetin cream and intraperitoneally injected with 30 mg/(kg·d) nuclear factor E2 related factor 2 (Nrf2) inhibitor ML385. The application amount was 2 mg/cm2. After 6 weeks of transdermal administration, the body weight, skin water content, skin antioxidant index, hydroxyproline (HYP) and hyaluronic acid (HA) levels were measured. The skin morphology was observed by HE staining. The transcriptional levels of COL1A1, COL3A1, matrix metalloproteinase (MMP) -1 and MMP-3 in skin were detected by RT-qPCR. The protein levels of Nrf2 (nucleus), Kelch-like ECH associated Protein 1 (Keap1) and heme oxygenase-1 (HO-1) in skin were detected by Western blotting. The results show that all three doses of isosinensetin increases skin water content, improves skin morphology, increases superoxide dismutase (SOD), catalase (CAT) and glutathione peroxidase (GSH-Px) levels, decreases malondialdehyde (MDA) levels, increases HYP and HA levels, increases COL1A1 and COL3A1 mRNA levels, decreases MMP-1 and MMP-3 mRNA levels, increases Nrf2 (nucleus) and HO-1 protein levels, and decreases Keap1 protein levels in skin aging mice (P<0.05). ML385 attenuates the anti-aging and antioxidant effects of isosinensetin (P<0.05). In short, transdermal administration of isosinensetin can improve the anti-aging and antioxidant ability of D-gal-induced skin aging mice by activating Nrf2 pathway.

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    Reviews
    Mechanism and research progress of chemical leukoderma induced by 4-substituted phenols
    Wanping Zhang, Qi Peng, Dongmei Zhang, Shilian Zheng, Wen Jiang, Lihao Gu
    2024, 54 (3):  320-328.  doi: 10.3969/j.issn.2097-2806.2024.03.011
    Abstract ( 71 )   HTML ( 10 )   PDF (1406KB) ( 100 )  

    4-substituted phenols are a class of organic compounds widely used in pharmaceuticals, pesticides, dyes, food additives and cosmetics. The application of 4-substituted phenols in cosmetics is mainly due to its structural similarity with tyrosine, which makes it have a unique effect of inhibiting tyrosinase activity and inhibiting melanin formation in the skin. Therefore, including chemical substances such as arbutin and resveratrol, there are many 4-substituted phenols used as whitening ingredients in cosmetics. However, 4-substituted phenols including hydroquinone also have certain safety risks. A large number of studies have shown that many 4-substituted phenols have melanocyte toxicity, and different substituents will also induce different pathways and toxicities of melanocyte toxicity. The improper use of them may induce the occurrence of vitiligo and leukoderma, causing harm to the consumers’ health. This article reviews the whitening and melanocyte toxicity mechanisms of 4-substituted phenols and hydroquinone, as well as the cases of leukoderma in different countries, in order to provide reference for the development of safer whitening chemicals.

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    Research progress on the evaluation methods of cosmetic after-sun repair efficacy
    Mengran Xu, Hua Zhao
    2024, 54 (3):  329-336.  doi: 10.3969/j.issn.2097-2806.2024.03.012
    Abstract ( 167 )   HTML ( 16 )   PDF (1123KB) ( 113 )  

    Human beings cannot avoid contact with UV rays in their daily lives, and the skin problems caused by UV radiation have become a common problem for people, which leads to a daily demand of the cosmetics claimed after-sun repair effect. The Cosmetics Efficacy Claim Evaluation Code requires that cosmetics with repair efficacy should be evaluated by the means of human efficacy evaluation tests for efficacy claims. In order to improve the research on the evaluation methods of cosmetic after-sun repair efficacy, and to meet the market demand for after-sun repair products from consumers, we provide research on the efficacy evaluation methods of after-sun repair cosmetics, and establish the basis for the establishment of an efficacy evaluation system for after-sun repair cosmetics. It briefly discusses the action mechanism of ultraviolet light on skin and after-sun performance, the action mechanism of after-sun repair products, the definition of repair efficacy and the regulatory requirements for the efficacy claims of repair cosmetics, the methods and research progress of clinical trials and in vitro tests on the efficacy of after-sun repair cosmetics (among which in vitro tests are divided into cell tests and animal tests), and provides an outlook on the establishment of an evaluation system for the efficacy of after-sun repair cosmetics.

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    Supervision and use analysis of sunscreen with potential endocrine disruption risk
    Na Ta, Mengxin Feng, Jiamin Gao, Fenglan Zhang, Gangli Wang
    2024, 54 (3):  337-343.  doi: 10.3969/j.issn.2097-2806.2024.03.013
    Abstract ( 214 )   HTML ( 4 )   PDF (1028KB) ( 97 )  

    The European Union has screened cosmetic ingredients with potential endocrine disrupting risks and established a priority assessment list for cosmetic ingredients, which includes four EU cosmetics directive approved sunscreens. This article focuses on the priority evaluation list of sunscreens, provides an overview and analysis of their regulatory status in countries (regions) such as the European Union and the United States, as well as their use in China. It also summarizes the reevaluation results of the European Union Consumer Safety Scientific Committee. After research and investigation, it is found that the regulatory limits for sunscreen in China on the priority evaluation list are basically consistent with those in the United States, Japan, and South Korea. However, some sunscreen limits are higher than the newly revised limits in the European Union, which may pose safety risks. It is recommended that regulatory authorities comprehensively evaluate the safety risks, actual usage, and industry development of the above-mentioned sunscreen agents, and further evaluate and refine regulatory limits to better ensure the safety of people’s makeup use.

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    Research progress of the correlation between sensory evaluation and instrumental analysis of cosmetics in O/W emulsion system
    Wenrui Zhou, Jianbiao He, Qian Jiao, Zidi Wang, Qianqian Su, Yan Jia
    2024, 54 (3):  344-352.  doi: 10.3969/j.issn.2097-2806.2024.03.014
    Abstract ( 111 )   HTML ( 7 )   PDF (1341KB) ( 74 )  

    With the rapid growth of the cosmetics industry, sensory evaluation is required when designing and optimizing products to meet consumers’ increasing needs and aspirations. Instrumental measurement methods such as rheology measurement and texture analysis have the advantages of simple operation, lower cost, objective and repeatability, which can control individual differences when using “people” as a tool for sensory evaluation. This article reviewed the literature on sensory evaluation and instrumental analysis and characterization of cosmetics in the domestic and overseas, introduced the definitions of various sensory attributes in sensory analysis, summarized instrument parameters and test methods strongly related to sensory attributes, and listed fitting equations for some sensory attributes and instrument parameters, providing a scientific basis for the formulation design and screening of cosmetics during R&D. However, there was an incomplete study of the correlation between certain sensory properties and instrument parameters, such as visual acuity, softness, smoothness, moisture, and other sensory properties. Subsequent studies should also consider the differences in sensory properties of consumers with different skin types after cosmetics use. The information in this paper would help readers to understand the correlation between sensory evaluation and instrumental parameters, providing a scientific reference for the development of cosmetics with good skin sensation.

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    Analytical methods and testing
    Determination of 14 kinds of α-hydroxy acids and hydroxy esters in cosmetics
    Liyuan Zhang, Linqi Yan, Qiaoyuan Cheng, Lvye Qi, Rong Wang, Liuqian Huang
    2024, 54 (3):  353-359.  doi: 10.3969/j.issn.2097-2806.2024.03.015
    Abstract ( 153 )   HTML ( 4 )   PDF (1221KB) ( 80 )  

    The study aimed to establish a method for simultaneous determination of 14 kinds of α-hydroxy acids and their esters in cosmetics by high performance liquid chromatography (HPLC),and the results were confirmed by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). HPLC was used for gradient elution with 0.05 mol/L diammonium hydrogen phosphate-methanol as the mobile phase. The analytes were separated on a Waters T3-C18 (4.6×250 mm, 5 µm) column and detected at the wavelengths of 214 nm. Quantification analysis was performed by the external standard method. HPLC-MS/MS was used for gradient elution with 0.1% formic acid-acetonitrile containing 0.1% formic acid as the mobile phase, and the analytes were separated on a Waters T3-C18 (2.1×100 mm, 1.8 µm) column. Qualitative analysis was performed by electronic spray ionization under a positive ion and negative ion mode with multiple reaction monitoring (MRM). The linearity of the 14 components in the concentration range is good, with the correlation coefficient r≥0.999. The average spiked recoveries of 14 compounds in 4 cosmetic matrices are all in the range of 85%-115%, and the relative standard deviations are all less than 5%. The limits of detections range from 1 μg/g to 150 μg/g. The limits of quantitation range from 3 μg/g to 450 μg/g. Seven batches of samples containing α-hydroxy acid and its ester were confirmed by HPLC-MS/MS and the results are positive. The results indicate that the method is simple, sensitive and accurate, and is suitable for the determination of 14 kinds of α-hydroxy acids and their esters in cosmetics.

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    Determination of 36 stimulants in cosmetics by ultra performance liquid chromatography-tandem mass spectrometry
    Wei Xu, Po Zou, Changyu Li, Ming Yang, Yan Lu, Huiliang Li
    2024, 54 (3):  360-368.  doi: 10.3969/j.issn.2097-2806.2024.03.016
    Abstract ( 94 )   HTML ( 6 )   PDF (1527KB) ( 87 )  

    An ultra performance liquid chromatography-tandem mass spectrometric (UPLC-MS/MS) method was developed for the simultaneous determination of 36 stimulants including anabolic agents, β2 agonists, glucocorticoids, irritants, and cannabinoids in cosmetics. In this study, pretreatment operation and instruments parameters were also optimized. Cosmetic samples were ultrasonically extracted by methanol, and then the separation of 36 stimulants was carried out on a Waters ACQUITY UPLC BEH C18 column (3.0 mm×150 mm, 1.7 μm) by gradient elution, using 0.1% acetic acid solution and methanol-acetonitrile (1∶9, by volume) as the mobile phase. The 36 target compounds were analyzed in positive and negative electrospray ionization mode under multiple reaction monitoring (MRM) mode. Meanwhile, the analytes were quantified by external standard method, and the linear regression analysis data show that there are good linear relationships for 36 target compounds in the mass concentration range of 1.0-20 ng/mL, with their correlation coefficients (r) greater than 0.995. The limits of detection (LOD) and limits of quantitation (LOQ) of the method are in the ranges of 1.0-3.0 μg/kg and 3.3-9.9 μg/kg, respectively. The recoveries for 36 target compounds in three kinds of matrix samples at three spiked levels are between 80.6% and 115.3%, with the relative standard deviations (RSD) of 0.5%-12.9% (n=5). The method is simple, rapid, high sensitivity, accurate and suitable for the rapid detection of many stimulants in cosmetics.

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