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Table of Content

    22 November 2022, Volume 52 Issue 11 Previous Issue    Next Issue
    Basic research
    Study on slow-release surfactant nanocarriers in low-permeability reservoirs
    Kang Wanli,Wang Kanghui,Li Zhe,Lv Wei,Yang Hongbin,Jia Ruxue,He Yingqi
    2022, 52 (11):  1147-1154.  doi: 10.3969/j.issn.1001-1803.2022.11.001
    Abstract ( 1820 )   HTML ( 23 )   PDF (1995KB) ( 235 )  

    To solve the serious adsorption problem of surfactant flooding in low-permeability reservoir, beeswax, TX-10 and deionized water were used as oil phase, surfactant and water phase to prepare nanoemulsions. The ultrasonic emulsification method at a temperature above the melting point of beeswax (61 ℃) was applied, and then the temperature was reduced to fix TX-10 inside the oil phase, and thus a slow-release surfactant nanocarrier was obtained. By means of UV-vis spectrophotometer, particle size analyzer, interfacial tensiometer and contact angle analyzer, the encapsulation rate and oil displacement properties of nanocarriers were measured. The results showed that, with the increase of TX-10 mass concentration, the average particle size of the nanocarriers was decreased first and then increased, and the minimum particle size was approximately 105 nm when the concentration was 5 000 mg/L, and the encapsulation rate for TX-10 was approximately 90%. At the formation temperature (65 ℃), the nanocarriers could reduce the interfacial tension between simulated oil and water to 3.24×10-2 mN/m and the surface tension to 23.3 mN/m, which was better than the TX-10 solution alone. Moreover, the nanocarriers behaved slow-release in the process of reducing interfacial tension. In addition, the nanocarriers could reverse the wettability of the surface of oleophilic core, which was similar to TX-10 solution. The static adsorption loss rate was less than 0.1%, which was more than ten times lower than that of TX-10 solution. At 30 and 65 ℃, the oil washing efficiency of the nanocarriers was 87.7% and 92.3%, respectively, which was 4% higher than that of TX-10 solution. The nanocarriers prepared in this study can carry surfactants to migrate in formation pores and release surfactants slowly when in contact with crude oil. The nanocarriers have anti-adsorption ability while ensuring the performance of surfactants, showing a good application prospect for enhanced oil recovery in low-permeability reservoirs.

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    Synthesis and performance study of C12-14 secondary alcohol ethoxylates
    Li Yingxue,Sun Yongqiang,Zhou Jingjie,Sun Jinyuan,Liang Huibin,Liu Yuqi
    2022, 52 (11):  1155-1161.  doi: 10.3969/j.issn.1001-1803.2022.11.002
    Abstract ( 1220 )   HTML ( 20 )   PDF (1169KB) ( 351 )  

    A secondary alcohol polyoxyethylene ether with EO addition number of 3, SAEO3, was synthesized by using KOH and CH3OK as catalysts in ethoxylation reaction. The catalytic activities of both catalysts were evaluated. The effects of different catalysts on the performance of SAEO3 (including surface properties, physical and chemical properties, application properties, etc.) were systematically investigated. The properties of SAEO3 synthesized in the laboratory were also compared with those of the commercially available product Secol-30. The conclusions are as follows: Compared with KOH catalyst, the reaction activity and product selectivity were higher when catalyzed by CH3OK for the ethoxylation of secondary alcohols. The physical and chemical properties of SAEO3 were similar to those of the commercially available Secol-30, and the cloud point of the secondary alcohol ethers catalyzed by CH3OK was higher than those of the other products. The cmc of SAEO3 was lower than that of the commercially available Secol-30. However, Secol-30 had better ability to reduce surface tension, which could reduce the surface tension of aqueous solution to 28.25 mN/m at low concentration. SAEO3 has no gel phase region and has superior detergency, so it can be used in concentrated detergent products.

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    Lecture of science and technology
    Common cosmetic preparation technologies (V)Artificial biological membrane: Liposomes
    Shi Jing,Feng Yun,Qi Xi,Xu Guiyun,Fan Jinshi
    2022, 52 (11):  1162-1168.  doi: 10.3969/j.issn.1001-1803.2022.11.003
    Abstract ( 1323 )   HTML ( 22 )   PDF (1340KB) ( 404 )  

    Liposomes, one of the most attractive nanocarriers, are spherical microvesicles that have an internal aqueous core surrounded with a single or multiple concentric lipid bilayers. The lipid formulations are made of naturally occurring lipids or synthetic lipids and surfactants not existing in biological systems. Liposomes resemble cell membrane in terms of structure and composition that are considered as a significant candidate for the improvement of drug delivery systems. Furthermore, liposomes suggest various advantages such as biocompatibility, high loading capacity, increasing half-life, low toxicity, good solubilization and stability of incorporating drugs and preventing the degradation of the medicine in the physiological environment. Besides medicine, liposomes have also been used in many other fields such as food and cosmetics. Herein, the composition, structure, classification, physicochemical properties and preparation methods of liposomes are introduced, respectively. The characteristics of liposomes dosage forms and the transdermal absorption mechanism vitally related to the application of liposomes in the medicine and cosmetics are also briefly presented. Meanwhile, the common applications of liposomes in medicine, food and cosmetics are outlined, as well as the future directions of liposomes research and development are pointed out.

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    Development and application
    Regulation of crystal form and morphology of gypsum during two-step preparation of KH2PO4 via Ca(H2PO42-H3PO4-K2SO4 system
    Ye Wencai,Wu Qin,Yi Yun,Yu Wen,Cao Jianxin
    2022, 52 (11):  1169-1178.  doi: 10.3969/j.issn.1001-1803.2022.11.004
    Abstract ( 2197 )   HTML ( 8 )   PDF (4158KB) ( 278 )  

    In Ca(H2PO42-H3PO4-K2SO4 system, α-calcium sulfate was made as a by-product during the production of KH2PO4 through regulating the two-step crystallization reaction including the crystallization of CaSO4·2H2O at lower temperature and the crystal transformation from CaSO4·2H2O to CaSO4·0.5H2O at higher temperature. The effects of reaction conditions on the crystal formation and morphology of CaSO4, the yields of phosphorus and potassium, and the decalcification rate in the two-step crystallization process were studied. The results showed that, the preparation parameters such as reaction temperature, reaction time, K2SO4 solution concentration, SO42- excess coefficient, CaO/P2O5 molar ratio and P2O5 content significantly influenced the morphology of CaSO4 crystal, the yields of phosphorus and potassium, and the decalcification rate. When the first-step reaction and crystallization was operated at 70 ℃ for 60 min and the second-step crystallization transformation was operated at 102 ℃ for 5.0 h under the conditions of K2SO4 concentration being 10%, SO42- excess coefficient of 1.2, CaO/P2O5 ratio of 0.20 and P2O5 content of 25%, the yield of potassium and the yield of phosphorus and the decalcification rate of filtrate were 98.35%, 91.43% and 89.74%, respectively. The crystal form of the gypsum sample thus prepared was α-CaSO4·0.5H2O, and the morphology was hexagonal conical short column. The 2-hour-flexural-strength and absolute dry compressive strength reached 5.70 MPa and 35.07 MPa, respectively, which matched with the α30 level of the α-high-strength gypsum industry standard. The purity of the produced potassium dihydrogen phosphate was higher than 80%.

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    Research on the application of glycerin and 1.3-butanediol in the preparation of cleansing oil by D-phase emulsification method
    Dong Leilei, Huang Tianyi, Cai Yichao, Duan Guolan, Wu Xu, Zhou Qianhui, Zhang Dongmei
    2022, 52 (11):  1179-1187.  doi: 10.3969/j.issn.1001-1803.2022.11.005
    Abstract ( 2036 )   HTML ( 35 )   PDF (2798KB) ( 368 )  

    The cleansing oil was prepared by D-phase emulsification method. PEG-20 glycerol triisostearate was selected as the emulsifier, glycerol or 1.3-butanediol was used as the co-emulsifier, and 10 kinds of oils in mineral oil, alkane and ester were selected. The effects of oils and polyols on the appearance, conductivity, microstructure and type of emulsion formed during D-phase emulsification were systematically analyzed. The research results show that: according to the ratio of fat∶emulsifier∶co-emulsifier (6∶3∶1), it is found that mineral oil (7#, 10#), ethylhexyl palmitate and two polyols can all form transparent cleansing oil system, but isohexadecane can only work with 1.3-butanediol to get the same system. By observing the appearance and electrical conductivity of the emulsion, it is found that the greater the interfacial tension between ester oils and glycerol, the higher the transparency of the formed system and the smaller the particle size. Compared with glycerin, 1.3-butanediol can improve the transparency of the microemulsion and the conductivity of the particles in the D-phase emulsification process, and it is easier to form a two-continuous phase structure, which can be used in a cleansing oil formulation system.

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    Evaluation of anti-wrinkle effect of neurotransmission inhibitory peptides by Caenorhabditis elegans
    Liu Han,Guo Chaowan,Chen Jie,Nie Yanfeng,Hu Lu,Wang Juan
    2022, 52 (11):  1188-1194.  doi: 10.3969/j.issn.1001-1803.2022.11.006
    Abstract ( 309 )   HTML ( 13 )   PDF (1805KB) ( 265 )  

    With the cosmetics industry entering the high-tech development period, people pay more attention to the maintenance of the skin, especially the sharp increase in the demand for skin texture smoothing and wrinkle desalinization. However, the efficacy evaluation of anti-wrinkle cosmetics or raw materials has the problems of long cycle, high cost and inability to achieve high-throughput detection. Therefore, it is of great significance for product development to establish a feasible and effective alternative detection model, in order to achieve the rapid evaluation of the wrinkle-removing efficacy of cosmetic raw materials. In this study, Caenorhabditis elegansC. elegans) was used as the model organism to test the inhibitory effects of several kinds of cosmetic peptides on neuromuscular synapses. The movement behaviors of the treated C. elegans were observed and two main enzymes function in neuromuscular junctions, the Acetylcholinesterase (AChE) and the Calcineurin (CaN), were also tested. The results show that, after treatment with all tested peptides (including scorpion venom, snake venom peptide, conotoxin and the compound peptide by scorpion venom and conotoxin), the movement behavior of C. elegans (head swinging and body bending) is inhibited to a certain extent (9%-33%). And the tail muscles can not contract normally, showing the movement state of trailing and crawling. With the intervention of neostigmine methylsulfate, the body bending amplitude of the C. elegans after exercise injury recovers little, and the movement behavior of C. elegans is inhibited about 5%-17%. These data indicate that all of the tested peptides show strong inhibitory activities on normal synapse formation between motor neuron and muscle, with remarkably inhibiting the locomotor behavior of C. elegans. In addition, we further find that these peptides stimulate the overexpression of CaN while inhibiting the enzyme activity of AchE, thereby blocking the functions of neuromuscular junction, which leads to muscles relax and achieves the anti-wrinkle effects. Various types of neurosuppressive peptides have different targets and different action mechanisms for exerting anti-wrinkle activity. Compared with the anti-wrinkle polypeptide with a single target, the polypeptide raw material compounded by the red scorpion element and the cono peptide can exert more excellent anti-wrinkle activity. Furthermore, by testing the movement recovery ability of C. elegans, the head swing frequency of C. elegans recovers to the level of the blank group (P>0.05), which indicates that these neuroprotective peptides have no neurotoxicity to C. elegans, and are immediate and safe. In conclusion, the methods described in this study can provide scientific reference for the development and efficacy verification of anti-wrinkle ingredients for skin care products.

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    Chlorogenic acid ameliorates UVB-induced HaCaT inflammation through SIRT6
    Wu Simin,Man Jiaxu,Yuan Mei,Gao Ziqi,Wang Dongxue,Zhang Dongying
    2022, 52 (11):  1195-1201.  doi: 10.3969/j.issn.1001-1803.2022.11.007
    Abstract ( 266 )   HTML ( 15 )   PDF (1785KB) ( 221 )  

    The aim of the study was to investigate the regulatory effect and mechanism of chlorogenic acid (CGA) on UVB-induced inflammatory response in HaCaT cells. HaCaT cells exposed to UVB were treated with CGA, and the protective effect of CGA on HaCaT cells damaged by UVB was detected by crystal violet staining. Changes in intracellular TNF-α content were detected by enzyme-linked immunosorbent assay, the antioxidant capacity of CGA in and out of the cells was detected by ABTS, DPPH, and FRAP assay, MDA content in the cells was detected by malondialdehyde kit, changes in total intracellular reactive oxygen species were detected by CM-H2DCFDA staining, and the relative expression of SIRT6, TNF-α, P-AKT, P-AMPK, AMPK, β-Tubulin proteins were detected by Western blot assay. Crystal violet staining and microscopy indicate that 100 and 150 μmol/L CGA are protective for 21.6 mJ/cm2 UVB-treated HaCaT cells. Enzyme-linked immunosorbent assay results indicate that CGA treatment significantly reduces TNF-α expression (P<0.01). CGA has good free radical scavenging ability both inside and outside cells, and is able to effectively reduce the UVB induced production of MDA and ROS. CGA can significantly inhibit the upregulation of SIRT6 expression caused by UVB, thereby reducing the phosphorylation level of AKT, activating AMPK and then reducing the expression of TNF-α, and alleviating the inflammatory response of the cells. CGA can inhibit SIRT6 to reduce the inflammatory response of UVB-induced HaCaT cells and reduce UVB-inflicted cellular oxidative stress with strong anti-cutaneous photoaging activity.

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    Inhibitory effects of seven plant essential oils against Malassezia furfur and the antimicrobial mechanism of Cinnamomum camphora essential oil
    He Yuan,Li Ziqiang,Sun Weijie,Ma Shumei,Liu Li
    2022, 52 (11):  1202-1207.  doi: 10.3969/j.issn.1001-1803.2022.11.008
    Abstract ( 465 )   HTML ( 20 )   PDF (2048KB) ( 308 )  

    By comparing the inhibitory activities of seven essential oils against Malassezia furfur, the most effective ones were selected and further analyzed. The essential oils with the best antibacterial effects were determined by K-B disk diffusion method and broth microdilution method. In addition, the volatile components of the essential oils with the best antibacterial effects were identified by gas chromatography-mass spectrometry (GC-MS), and further correlation analysis was performed between the main chemical components and the activity against Malassezia furfur. Then, the morphological changes of Malassezia furfur were observed by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Finally, the effect of Malassezia furfur on cell apoptosis was detected by flow cytometry. The results showed that, Cinnamomum camphora essential oil was more active against Malassezia furfur than the essential oils from Osmanthus fragrans, Citrus limon, Lavandula angustifolia, Rosmarinus officinalis, Melaleuca alternifolia, and Citrus bergamia. A total of 14 chemical components were identified by GC-MS, and the inhibitory activity against Malassezia furfur was derived from 3-carene, terpinene-4-ol, α-terpinene, terpinolene; SEM showed that Cinnamomum camphora essential oil caused mild damage to the cells of Malassezia furfur, and the local cell membrane was depressed; TEM showed that Cinnamomum camphora essential oil caused the plasmolysis of Malassezia furfur, and the intracellular matrix was lightened. Cinnamomum camphora essential oil significantly increased the apoptosis of Malassezia furfur. In conclusion, Cinnamomum camphora essential oil has a significant inhibitory effect against Malassezia furfur by destroying the cell wall and cell membrane.

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    Structural analysis and hypoglycemic activity analysis of polysaccharides from Acanthopanax sessiliflorus
    Yang Yongpeng,Xiu Yuwu,Huang Weizhi
    2022, 52 (11):  1208-1213.  doi: 10.3969/j.issn.1001-1803.2022.11.009
    Abstract ( 155 )   HTML ( 7 )   PDF (1220KB) ( 172 )  

    The aim was to isolate and purify the polysaccharide components in Dangsengwujia, analyze the structure of the components through experiments, and analyze their antioxidant bioactivity. The polysaccharides named ASP were isolated and purified from the stems of Acanthopanax sessiliflorus, and their structural characteristics were studied and analyzed by high performance liquid chromatography, gas chromatography-mass spectrometry, Fourier transform infrared, ultraviolet-visible spectroscopy, 1H NMR and 13C NMR. The antioxidant activities and iron ion reduction ability of polysaccharide of ASP to 1,2-dipicyl-2-trinitrophenylhydrazine (DPPH), and 2,2-biazo-bis (3-ethyl-benzothiazol-6-sulfonic acid) ammonium salt (ABTS) were evaluated. The experimental results show that the polysaccharide of ASP is composed of mannose, glucose, galactose and arabinose, and its structure is mainly composed of pyranose rings. It can effectively scavenge DPPH, ABTS cation free radicals, reduce iron ions, and show a certain antioxidant capacity. The polysaccharides from ASP have good antioxidant bioactivity.

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    Experimental study on dense foam toothpaste
    Yi Rui,Xu Chunsheng
    2022, 52 (11):  1214-1220.  doi: 10.3969/j.issn.1001-1803.2022.11.010
    Abstract ( 229 )   HTML ( 10 )   PDF (1774KB) ( 265 )  

    The pH, foam volume and foam stability of alkyl glucoside (APG) compounded with six other foaming agents including sodium dodecyl sulfate (K12), sodium lauroyl sarcosinate (LS-30), sodium cocoyl glutamate, sodium methyl cocoyl taurate, biological glycolipid and capryl/capramidopropyl betaine in a ratio of 1∶1 in the toothpaste ternary solution of common proportion were studied. Based on this, ordinary calcium carbonate toothpaste and silica toothpaste were made. The foam volume of each toothpaste was measured by Ross-Miles foam analyzer. The pH of each toothpaste was also measured. The foam height of the toothpaste during the stirring process with agitator was measured. Then, the dense foam test was carried out to compare with the toothpaste using sodium dodecyl sulfate as foaming agent. In addition, the foam volume and foam height of several commercial high-foam toothpastes were tested to compare with the self-made silica toothpastes. By these methods above, the foam properties of the self-made toothpaste containing APG compounded with other foaming agents were evaluated. The results indicate that, when APG is combined with K12, LS-30, sodium methyl cocoyl taurate and biological glycolipid, respectively, the foam amount, foam stability and foaming speed are increased for corresponding calcium carbonate and silica toothpastes. Meanwhile, the pH values of toothpastes are in the ideal range under other components’ buffering.

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    Reviews
    Establishment and prospects of the database for safety information on cosmetic ingredients in China
    Su Zhe,Hu Kang,Wang Gangli,Lu Yong
    2022, 52 (11):  1221-1228.  doi: 10.3969/j.issn.1001-1803.2022.11.011
    Abstract ( 1347 )   HTML ( 21 )   PDF (1003KB) ( 262 )  

    With the newly revised Regulations on the Supervision and Administration of Cosmetics, the National Medical Products Administration (NMPA) has established new regulations and an improved technical system for cosmetics. NMPA has strengthened ingredient management and safety assessment of cosmetics. NMPA has put forward the requirements for submission of the safety information of cosmetic ingredients. On the basis of relevant regulations and practical needs in supervision, the National Institutes for Food and Drug Control (NIFDC) has studied ingredient management, including classification, key features and basic information of ingredients, identification, characteristic indexes, risk information and control, and use of safety information, and accordingly, NIFDC has built a “cosmetic ingredient information platform” for the submission and management of such safety information. In future, with collecting, utilizing, and analyzing of the safety information of cosmetic ingredients, as well as with integrating those databases related to cosmetic regulations and technical standards, NMPA and NIFDC will build a scientific and efficient “database for safety information on cosmetic ingredients” in China, which will provide strong big-data support in technical work and will continuously improve the supervision and safety evaluation for cosmetics.

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    Application of visual culture integration and psychological driving factors in cosmetic packaging design
    Zheng Wei
    2022, 52 (11):  1229-1235.  doi: 10.3969/j.issn.1001-1803.2022.11.012
    Abstract ( 169 )   HTML ( 5 )   PDF (1154KB) ( 165 )  

    High-quality cosmetic appearance and packaging design can effectively increase consumers’ brand trust and enhance the sales and brand awareness of cosmetics. Herein, the combination of visual culture with psychological driving factors was integrated into cosmetic appearance and packaging design. The embodiment of visual culture in cosmetic appearance and packaging design was discussed from three aspects, i.e., society, consumption concept and profit space; in addition, the embodiment of psychological driving factors in the visual design of cosmetic appearance and packaging was discussed from the aspects of motivation, and the driving forces from consumer demand, practicality and experience. In view of the research results above, a new strategy of cosmetic packaging design was proposed. As guided by the visual culture design to drive consumer psychology, the visual culture design can be carried out from multiple psychological driving factors to attract consumers’ attention and interest, arouse consumers’ desire for purchase, promote consumers’ purchase behavior and provide new ideas for cosmetic packaging design.

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    Analytical methods and testing
    Determination of ectoine and hydroxyectoine in fermentation broth by high performance liquid chromatography
    Liu Zihan,Guo Qiushuang,Zhou Chao,Sun Yang,Li Hua,Liu Yupeng
    2022, 52 (11):  1236-1240.  doi: 10.3969/j.issn.1001-1803.2022.11.013
    Abstract ( 459 )   HTML ( 18 )   PDF (1161KB) ( 387 )  

    A method was developed for the determination of ectoine and hydroxyectoine in fermentation broth samples of moderately saline bacteria using high performance liquid chromatography (HPLC). Samples were extracted using ethanol extraction, and ectoine and hydroxyectoine standards were dissolved and diluted in ultrapure water. VertexTM NH2 (4.6×250 mm, 5 μm) liquid chromatographic column was used to analyse ectoine and hydroxyectoine in the fermentation broth of moderately halophilic bacteria. Waters 1515 high performance liquid chromatograph with ultraviolet (UV) detector was selected to compare the different detection conditions. The chromatographic conditions were optimized by using acetonitrile (70%) as the mobile phase with a column temperature of 30 ℃, a detection wavelength of 210 nm and a flow rate of 0.8 mL/min. The linearity of ectoine and hydroxyectoine in the fermentation broth samples is good in their respective ranges. The average recoveries of the two samples are in the range of 99.2% to 102%, the precision deviations are in the range of 1% to 2%, the limit of detection is 1.5 μg/mL, the limit of quantification is 5 μg/mL and the separation degree is 1.70. The method is suitable for the separation and determination of ectoine and hydroxyectoine in fermentation broth and for the quantitative analysis of ectoine and hydroxyectoine under laboratory conditions.

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    Study on the detection of preservatives in infant and adult skin care products by HPLC
    Liu Hui,Li Li,Liu Tingyuan,Xu Qinke,Sun Ying,Guo Zhaohui
    2022, 52 (11):  1241-1247.  doi: 10.3969/j.issn.1001-1803.2022.11.014
    Abstract ( 171 )   HTML ( 9 )   PDF (1165KB) ( 192 )  

    The situation of addition of preservatives in infant and adult skin care products was studied, which is expected to accumulate scientific data for the safety monitoring and quality research of preservatives therein. 12 preservatives were detected for 140 batches of skin care products based on the method for 23 preservatives as shown in the “Technical Specification for Safety of Cosmetics “ (2015 edition) (Announcement No. 17 of 2021, National Medical Products Administration). The test results were statistically analyzed. The results showed that, the linear correlation coefficients were all greater than or equal to 0.996 9, the recovery rate of standard addition was 91%-104%, and the RSD was less than 5.0%. There were many samples from Guangdong Province and Shanghai, and no over-limits or prohibited components were detected. Phenoxyethanol, methylparaben and propylparaben are more frequently used; phenoxyethanol is frequently used in infant skin care products; methylparaben and propylparaben are commonly compounded in retention products, and the frequency of use in adult skin care products is high; the mixture of methylchloroisothiazolinone, methylisothiazolinone, magnesium chloride and magnesium nitrate has only been added to rinse-off products. There are a maximum of 1-3 components in a single batch of infant skin care products of 54 batches, and a maximum of 1-3 components in a single batch of samples in adult skin care products of 62 batches. The amount of preservatives in infant skin care products (0-2.3%) is significantly higher than that of adult skin care products (0.000 16%-1.19%). In this test, presence of 1-3 preservatives in infant and adult skin care products has become the mainstream, and phenoxyethanol, methylparaben and propylparaben are the main preservative components.

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    Determination of preservatives in toothpaste by high performance liquid chromatography
    Zhang Xiaoping,Wang Shifang
    2022, 52 (11):  1248-1253.  doi: 10.3969/j.issn.1001-1803.2022.11.015
    Abstract ( 190 )   HTML ( 9 )   PDF (1154KB) ( 176 )  

    In order to manage and limit the types and amounts of preservatives in toothpaste and to improve the quality of toothpaste, a method for determining the content of preservatives in toothpaste by high performance liquid chromatography was studied. The mixed standard solution of preservatives was prepared with five reagents including methylparaben, ethylparaben and benzoic acid, and the toothpaste samples were treated with solutions such as acetonitrile. Sodium dihydrogen phosphate solution, methanol and acetonitrile mixed solution were used as mobile phases. The mixed standard solution and toothpaste samples were measured under the conditions that the column temperature, injection volume and flow rate were room temperature, 5 μL and 1.5 mL/min, respectively. A standard curve was drawn according to retention time and area of chromatographic peak of mixed standard solution. The results show that: under the condition that the ratio of sodium dihydrogen phosphate solution, methanol and acetonitrile in the mobile phase is 55∶25∶20, the separation degree of the mixed standard solution is the highest. The recovery rate of various preservatives fluctuates between 88.68% and 99.61%, and the relative standard deviation fluctuates between 0.39% and 2.44%. The repeatability test results meet the needs of practical applications.

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    Determination of menthol and menthyl lactate in cosmetics by GC-MS
    Xiong Zhi,Shi Jiajia,He Quanquan
    2022, 52 (11):  1254-1258.  doi: 10.3969/j.issn.1001-1803.2022.11.016
    Abstract ( 270 )   HTML ( 8 )   PDF (1064KB) ( 386 )  

    The differences in qualitative and quantitative analysis between menthol of different configurations were compared. A method for simultaneous determination of menthol and menthyl lactate by GC-MS was established. The injection mode, extraction solvent, extraction time, column, split ratio and other parameters were studied. Samples were ultrasonically extracted by methanol, separated by a VF-WAXms column (30 m×0.25 mm×0.25 μm), detected with selected ion monitoring (SIM) scanning mode by direct liquid introduction, and quantified by external standard method. The results show that, there are no significant differences in response, retention time and SCAN mass spectra for menthol with different configurations; the linearity is good for menthol and menthyl lactate in the range of 0.1-100 mg/L, with the correlation coefficient above 0.999; the detection mass concentrations are 0.009 and 0.002 mg/L, the detection limits are 0.9 and 0.2 mg/kg; the quantification mass concentrations are 0.027 and 0.006 mg/L, and the quantification limits are 2.7 and 0.6 mg/kg; the recovery rates of the spiked standards are 96.3%-100.7% with the relative standard deviations of 1.9%-3.5%. Four products (a facial cleanser, two shampoos and a hair conditioner) were tested by this method. This method is simple, sensitive, and accurate, and it is suitable for the determination of menthol and menthyl lactate in cosmetics.

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