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    22 April 2022, Volume 52 Issue 4 Previous Issue    Next Issue
    Basic research
    Determination of high-molecular-weight fatty alcohol polyoxypropylene-polyoxyethylene ether carboxylates
    Ran Lijun,Chen Qi,Chen Zhao,Cui Zhenggang
    2022, 52 (4):  345-354.  doi: 10.3969/j.issn.1001-1803.2022.04.001
    Abstract ( 301 )   HTML ( 125 )   PDF (1494KB) ( 323 )  

    Fatty alcohol polyoxypropylene (PO)-polyoxyethylene (EO) ether carboxylates (APEC) with relatively large molecular weight (1 500~3 000) are excellent surfactants for enhanced oil recovery due to their good tolerance to high temperature and high salinity. However, the quantitative analysis of this type of surfactants is still a problem. For example, using the typical two-phase titration in alkaline media with bromcresol green as indicator gives significantly underestimated results. The lack of an accurate and precise analytic method has brought difficulty to relevant formulation and quality control in industrial production. Herein, the applicability of the typical two-phase titration method in alkaline media with bromcresol green as indicator to the high-molecular-weight APEC was examined and a new method based on colorimetry was proposed. For the high-molecular-weight APEC synthesized, a linear calibration curve indicative of the relationship between the surfactant concentration in aqueous phase and the absorbance of chloroform phase at 630 nm equilibrated with the aqueous phase after two-phase extraction could be obtained, in which the purified product was used as standard sample, Hyamine 1622 was used as cationic surfactant, bromcresol green was used as indicator, and chloroform was used as extraction agent of the color. By these means, the content of APEC in industrial products can be determined and the conversion can also be obtained. Specifically, the minimum concentration detectable of the APEC in aqueous phase can be as low as 10-6 mol/L, and the recovery can be higher than 97%.

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    Lecture of science and technology
    Preparation, properties and applications of natural biomass materials (Ⅳ) Stable multipurpose seaweed gel: agar
    Qi Xi,Fan Jianru,Feng Yun,Xu Guiyun,Fan Jinshi
    2022, 52 (4):  355-362.  doi: 10.3969/j.issn.1001-1803.2022.04.002
    Abstract ( 314 )   HTML ( 16 )   PDF (1377KB) ( 444 )  

    Agar is a kind of seaweed polysaccharide extracted from marine red algae, and it is also one of the most widely used algal gels in the world. Agar consists of neutral agarose and charged agaropectin, in which agarose is based on a disaccharide backbone of 1,3-linked -β-D-galactopyranose and 1, 4-linked 3, 6 anhydro-ɑ-L-galactopyranose repeating units, while agaropectin possesses molecular structure similar to that of agarose, with some sulfate groups, methoxyl groups and pyruvate groups linked to the galactopyranose in varying degrees. Due to its excellent properties such as gelling, non-toxicity, stability, thickening, transparence, suspending, shaping, as well as the more and better functions that could be obtained by the degradation, oxidization, carboxyalkylation, hydroxyalkylation and hydrophobization of the active groups including hydroxy groups and glycosidic bonds in the agar molecules, agar and its derivatives have been extensively used in food, biology, medicine, cosmetics, agriculture and other fields. Herein, the name, source and molecular structure of agar, the physical properties, conventional and improved production methods, and typical modification technology of agar, as well as the current research and application status of agar and its derivatives were introduced. The current problems, research trend and development prospect of agar and its modified products were also pointed out.

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    Development and application
    Effects of nano-silver on the surface activity of triethanolammonium cocoyl glutamate
    Yu Dongxiu,Jin Xiangxin,Liu Jiaxin,Li Junlang
    2022, 52 (4):  363-369.  doi: 10.3969/j.issn.1001-1803.2022.04.003
    Abstract ( 227 )   HTML ( 14 )   PDF (1589KB) ( 295 )  

    The mixed system of 50 mg/kg nano-silver and triethanolammonium (TEA+) cocoyl glutamate was prepared by green chemical method using cocoyl glutamic acid as raw material. The effects of nano-silver on the critical micelle concentration (cmc), foaming properties, pH, Krafft point and wetting properties of the mixed system were studied by measurement of conductivity, surface tension and contact angle and by Ross foam analyzer. The results showed that nano-silver could enhance the foaming performance and foam stability of the system. With the increase of the amount of nano-silver, the cmc was first decreased and then increased, and the foaming performance was first enhanced and then decreased, while no significant effects on pH, Krafft point or wetting performance were observed. In this experiment, 5% of 50 mg/kg nano-silver had excellent synergistic effect on the surface activity of TEA-cocoyl glutamate. The mechanism of nano-silver was explored by UV-Vis, FT-IR and Zeta potential. The results showed that the nano-silver did not dissociate in the system. And with the increase of its dosage, the nano-silver tended to adsorb near the N-H bond by electrostatic interaction, resulting in a coordination effect. The physical adsorption of nano-silver in this mixed system was greater than chemical adsorption. It was also found that with the increase of the amount of nano-silver, the absolute value of Zeta potential of the mixed system was decreased, but the absolute value of Zeta potential was greater than 50 mV, indicating that the mixed system of nano-silver/cocoyl glutamic acid triethanolamine had good stability.

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    Study on multifunctional hair care efficacy of sodium hyaluronate
    Hu Chenyu,Qu Wenjie,Guo Xueping,Xu Guixin,Zou Songyan,Wang Jing
    2022, 52 (4):  370-375.  doi: 10.3969/j.issn.1001-1803.2022.04.004
    Abstract ( 1058 )   HTML ( 24 )   PDF (1435KB) ( 382 )  

    Sodium hyaluronate is widely used in medicine and other fields because of its moisturizing, anti-inflammatory, antibacterial, antiallergic and repairing effects. It has also been widely used as a favorable bioactive ingredient in cosmetics. However, the research on sodium hyaluronate in cosmetics has been focused on its application in skin care, while few study has been carried out on the hair care efficacy thereof. Particularly, the hair care efficacy of sodium hyaluronate with different molecular weight has not been reported until now. Herein, the hair care efficacy of five kinds of sodium hyaluronates with different molecular weight and structure was systematically studied based on the characterization of mechanical properties, combability, friction force, moisture content and smoothness of hair. Experimentally, natural hair and highly-damaged hair were treated by leave-on products containing 0.5% (w/%) sodium hyaluronate. The results indicated that hydrolyzed sodium hyaluronate with lower molecular weight (30-50 kDa and less than 5 kDa) exhibited more significant multifunctional hair care effects. In detail, the tensile strength and elastic modulus of damaged hair can be significantly enhanced (up to 10%), and the combing work and friction force of the hair can be reduced by over 20%. Moreover, the sodium hyaluronate treatment leads to improved moisturizing and anti-frizz property of hair. The water loss curve of hair bundle treated with sodium hyaluronate at 65 ℃ was significantly lower than that of the control group. And in the high-humidity environment, the change of hair bundle projection area after sodium hyaluronate treatment was also significantly less than that of the control group. The hair care effects of sodium hyaluronate could be possibly attributed to its interaction with hair keratin, and the effectiveness of low-molecular-weight sodium hyaluronate could be related to their enhanced penetration into hair fibers. In addition, the experiment with fluorescently labeled sodium hyaluronate directly proved that low-molecular-weight sodium hyaluronate could penetrate into the hair fibers. This study provides theoretical basis and data support for the application of sodium hyaluronate in hair care products.

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    Study on the preparation and antibacterial properties of antibacterial hand sanitizers containing dodecyl dipropylene triamine
    Lin Xianjia,Cao Yan,Luo Wenyi,Lin Zhen,Zhang Zhiguo,Wen Yanmei
    2022, 52 (4):  376-382.  doi: 10.3969/j.issn.1001-1803.2022.04.005
    Abstract ( 523 )   HTML ( 21 )   PDF (1140KB) ( 279 )  

    The hand sanitizers containing dodecyl dipropylene triamine (DDT, antibacterial component) were prepared with the thickening systems such as AES-6501-NaCl, CAB-35-AES-NaCl, acrylic acid-2-acrylamide-2-methylpropanesulfonic acid, 6502-NaCl (Na2SO4), and polyethylene glycol 6000 distearate (638). The same mass fraction of DDT was added to these systems respectively. Then the viscosity and transmittance were investigated to judge the compatibility of these thickening systems with DDT. Single factor experiments were further carried out and the formula was optimized. The hand sanitizer containing DDT was thus prepared. Then the properties of the hand sanitizer were tested, including stability, viscosity, active substance content, pH value, foam height and bactericidal performance. The experimental results show that, the 638 system is compatible with DDT, while other thickening systems are not compatible with DDT. After high-temperature and low-temperature stability tests, the antibacterial hand sanitizer containing DDT shows no phase separation, no precipitation and no obvious color change, indicating that it has good stability. The viscosity is 2 767 Pa·s, which proves that the hand sanitizer can stay on the skin for a long time. The average value of active substance content is 10.2% and the pH value is 5.5, which all meet the national standard. The average bactericidal rates of the hand sanitizer against Escherichia coli and Staphylococcus aureus in 2 minutes were 97.63% and 98.96%, respectively.

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    Effect of Staphylococcus epidermidis fermented extract on human skin barrier
    Tie Hang,Lv Yufeng,Zhang Yang,Xu Liang,Yan Yan
    2022, 52 (4):  383-389.  doi: 10.3969/j.issn.1001-1803.2022.04.006
    Abstract ( 297 )   HTML ( 13 )   PDF (1559KB) ( 414 )  

    A large number of studies have shown that Staphylococcus epidermidis (SE), one of the normal microflora colonized in human skin and mucous membrane, plays a positive role in human skin barrier health. Here we reveal a new mechanism which a product of Staphylococcus epidermidis can enhance the skin barrier function. This enhancement is mediated by a Staphylococcus epidermidis fermentation extract isolated from healthy human skin in our laboratory, and acts on keratinocytes (KC) as well as 3D epidermal model triggered through Toll-like receptor (TLR) 3, filaggrin (FLG) and loricin (LOR), respectively. The effect of SE fermentation extract on human keratinocytes was detected by Real Time Cellular Analysis (RTCA). Polyinosinic-polycytidylic acid (poly (I:C)) and lipopolysaccharide (LPS) were used to stimulate KC cells respectively, causing TLR3 and TLR4-mediated inflammatory response models, and then added SE fermentation extract to study the inhibitory effects of SE fermentation extract on the inflammatory KC cells. Finally, sodium lauryl sulfate (SLS) was used to stimulate the 3D epidermal model to construct a damaged skin model, and to study the effect of SE fermentation extract on the expression of filaggrin (FLG) and loricin (LOR) in the damaged skin model. The results show that 1% (φ) SE fermentation extract acts on KC cells for 100 hours, and no obvious cytotoxicity is seen, which has a certain protective effect on cell activity. From this we can predict that SE may have some effect on the function of human epidermis, for example, enhancing the skin barrier function. SE fermentation extract can inhibit the inflammatory response mediated by TLR3, but has no obvious inhibitory effect on the inflammatory response mediated by TLR4. We speculate that Staphylococcus epidermidis fermentation extract may affect the inflammatory response of keratinocytes through the negative regulation of TLR signal. The results of the 3D skin model show that the SE fermented extract can effectively increase the FLG and LOR content in the damaged barrier. These findings show that Staphylococcus epidermidis, as a resident bacteria of human skin, can modulate specific cutaneous inflammatory responses and enhance the skin barrier function through research on keratinocytes and 3D epidermal model after wounding.

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    Study on the activity of flavonoids in the fermentation broth of Chinese wolfberry branches
    Zhang Yuzhi,Zhao Dan,Wang Dongdong,Zhang Jiachan,Wang Changtao,Li Meng
    2022, 52 (4):  390-395.  doi: 10.3969/j.issn.1001-1803.2022.04.007
    Abstract ( 261 )   HTML ( 14 )   PDF (1314KB) ( 326 )  

    The branch of Lycium barbarum was taken as the main research object. Flavonoids were extracted from Chinese wolfberry branches by microbial fermentation and alcohol extraction, respectively. The results show that the content of flavonoids obtained by microbial fermentation is higher than that obtained by alcohol extraction, indicating that microbial fermentation can improve the content of active components. 1,1-diphenyl-2-trinitrophenylhydrazine (DPPH) colorimetry was used to detect the DPPH scavenging ability of the fermentation broth and alcohol extract of barbarum. The results show that the 50% inhibition concentration (IC50) of DPPH free radical scavenging efficiency of the fermentation liquid and alcohol extract of Chinese wolfberry branches are 20.61 and 25 μg/mL, respectively, indicating that the microbial fermentation liquid has a stronger DPPH free radical scavenging ability. Macroporous adsorption resin was used to isolate and purify flavonoids from the fermentation liquid of Lycium barbarum. The level of reactive oxygen (ROS) in normal human somatic cells is controlled in a very low range, but in an illness state, ROS production can rapidly increase and cause human abnormalities or tissue lesions. The content of ROS in fibroblasts was determined, and the results show that flavonoids from Lycium barbarum has a good scavenging effect on ROS. MTT assay was used to detect the toxicity of the purified flavonoids to fibroblasts (HDF) and human immortalized keratinocytes (HaCaT). The results show that the survival rate of cells is the highest when the mass concentration of 1 μg/mL of flavonoids is added, so 1 μg/mL of flavonoids is selected as the final concentration. The effects of 2 h treatment of the flavonoids on the content of inflammatory cytokines were investigated, the results show that protein antibody TNF-AIP3 expression is down-regulated; IL6 is up-regulated, and IL8 (CXCL8) expression is down-regulated. IL-6, IL-8 and TNF-AIP3 play an important role in inflammatory response. When inflammation occurs, the expression levels of these three factors change, further promoting the inflammatory response and promoting the progression of the disease. Therefore, using microbial fermentation to extract the branches of Lycium barbarum and add them to pharmaceutical industry or food production can not only reuse resources, but also have certain anti-inflammatory and anti-oxidation effects.

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    Preparation and characterization of magnetic solid acid catalyst Fe3O4/C-SO3H
    Yu Hongmei,Hua Ping,Li Jianhua,Qian Feng
    2022, 52 (4):  396-403.  doi: 10.3969/j.issn.1001-1803.2022.04.008
    Abstract ( 231 )   HTML ( 11 )   PDF (1440KB) ( 336 )  

    Fe3O4/C-SO3H was a magnetic carbon-based solid acid catalyst. It was prepared with Fe3O4, biomass carbon and sulfonic acid source, in which Fe3O4 was the magnetic core and biomass carbon (glucose, starch, sucrose) was the raw material. Firstly, Fe3O4/C was prepared by the carbonization reaction taken place between Fe3O4 and biomass. Then, sulfonation of Fe3O4/C with p-toluenesulfonic acid was carried out, and thus Fe3O4/C-SO3H was prepared. The synthesis of octyl glucoside was used as a probe reaction. The activity of the catalyst was measured by the conversion of glucose and the catalyst acid content. The influencing factors such as biomass carbon type, carbonization temperature, carbonization time, acid type, sulfonation temperature and sulfonation time were investigated. The catalyst was characterized by FT-IR, XRD, TG, SEM and Vibrating Sample Magnetometer (VSM). The results show that, the optimum preparation conditions of Fe3O4/C-SO3H are as follows: Starch is the best biomass carbon source among glucose, starch and sucrose; the mass ratio of Fe3O4 to starch is 1:10; carbonization temperature is 190 ℃; carbonization time is 8 h; among the three sulfonic acid sources (p-toluenesulfonic acid, dodecylbenzene sulfonic acid and concentrated sulfuric acid), p-toluenesulfonic acid is the best; the mass ratio of Fe3O4/C to p-toluenesulfonic acid is 1:0.6; the sulfonation temperature is 250 ℃; the sulfonation time is 4 h. Under the optimized conditions, the acid content of the catalyst is 1.17 mmol/g, and the glucose conversion is 97.9%. XRD results show that the crystal structure of magnetic Fe3O4 particles does not significantly change after carbonization and sulfonation, and the catalyst still retains good magnetic properties. FT-IR analysis shows that sulfonic groups are successfully loaded on the carrier Fe3O4/C. Thermogravimetric analysis shows that Fe3O4/C-SO3H has good thermal stability below 300 ℃. SEM shows that magnetic Fe3O4 particles are irregular spherical particles with uniform size distribution and agglomeration. After carbonization, Fe3O4 are encapsulated by starch, and the particle size becomes larger, and there is a certain pore structure. The Fe3O4/C-SO3H catalyst also has a certain core-shell structure, and the particle size is approximately 30 nm. The VSM curves show that the magnetic strength of Fe3O4/C and Fe3O4/C-SO3H is much smaller than that of Fe3O4, but Fe3O4/C-SO3H can be separated from the system rapidly by simple magnetic attraction. It shows that the final magnetic properties of Fe3O4/C-SO3H meet the requirements of magnetic separation and recovery.

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    In vitro study on the protective effects of hyaluronic acid on eye irritation
    Geng Xue,Su Xinyu,Zhang Yanmei,Huang Siling,Zhao E,Zhu Qingfen
    2022, 52 (4):  404-409.  doi: 10.3969/j.issn.1001-1803.2022.04.009
    Abstract ( 382 )   HTML ( 14 )   PDF (1491KB) ( 266 )  

    Fluorescein leakage (FL) test and recombinant human corneal epithelial cell model eye stimulation (ET50) test were both took to investigate the protective effects of three different molecular weight hyaluronic acids (HA) including high, low and oligomeric on eye irritation. Firstly, seven verification substances in different stimulation levels including benzalkonium chloride (5%), 4-carboxy-benzaldehyde, promethazine hydrochloride, ethyl-2-methylaceto-acetate, glycerol, sodium lauryl sulfate (15%, w/%) and sodium hydroxide (10%, w/%) were used to verify the luciferin leakage test in our own laboratory. Then, fluorescein leakage test and in vitro artificial cornea model-eye stimulation ET50 test were both conducted to evaluate the inhibitory effect of three hyaluronic acids on eye irritation by the index of fluorescence leakage rate as well as cell survival rate. Fluorescein leakage test method is established successfully and is confirmed that 10 g/L mass concentration of hyaluronic acid can significantly reduce the increase of fluorescence leakage rate caused by 0.25 g/L mass concentration of benzalkonium bromide. What’s more, incubating for another 24 h after exposure to 10 g/L mass concentration of hyaluronic acid and 0.25 g/L mass concentration of benzalkonium bromide for 30 min, the cell survival rate does not change, but the morphological change of the cells can be observed tending to be normal under the microscope, compared to the cells treated by 0.25 g/L mass concentration of benzalkonium bromide only. Meanwhile, in vitro artificial corneal model-eye stimulation test confirms that oligo hyaluronic acid can significantly inhibit the decrease of cell survival rate which causes by methyl acetate at mass concentration of 20 g/L rather than 10 g/L. Accordingly, in vitro artificial corneal model-eye stimulation test (ET50) confirms that 10 g/L mass concentration of hyaluronic acid can significantly inhibit the decrease of cell survival rate and increase the ET50 value which is induced by 0.5 g/L mass concentration of benzalkonium bromide, but it falls flat on serious irritation induced by 10% (w/%) content of Brij35 solution. In conclusion, these results show that high, low and oligomeric molecular weight hyaluronic acid can all significantly reduce the irritation of ocular stimulation induced by mild positive substances, which provides a basis for the protective effect of hyaluronic acid, reveals a new prospect of the application of hyaluronic acid in cosmetics and presents a new method of efficacy evaluation on cosmetic raw materials.

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    Application and properties of the polysaccharide from red pulp pitaya stem in hand creams
    Tang Yayuan,He Xuemei,Sun Jian,Wei Zhen,Li Changbao,Liu Guoming
    2022, 52 (4):  410-417.  doi: 10.3969/j.issn.1001-1803.2022.04.010
    Abstract ( 237 )   HTML ( 9 )   PDF (1438KB) ( 250 )  

    The structural characteristics of pitaya stem polysaccharide (PSP) were analyzed. PSP was used as raw material to study its effects on hand creams. The PSP was extracted by hot water extraction and alcohol precipitation method. The total carbohydrate content of PSP was determined by anthrone-sulfuric acid method, and the uronic acid content of PSP was determined by sulfuric acid-carbazole method. The monosaccharide composition of PSP was analyzed by high performance liquid chromatography with diode array detector (HPLC-DAD) after 1-phenyl-3-methyl-5-pyrazolone derivatization (PMP). Different concentrations of PSP were used to prepare hand cream samples. The antioxidant capacity, moisturizing ability and rheological properties of the hand cream samples were evaluated in vitro. The total carbohydrate content of PSP is (346.88±9.05) mg/g and the uronic acid content of PSP is 38.76%±1.99%. The PSP consists of mannose, rhamnose, galacturonic acid, glucose, xylose, galactose and arabinose in the following molar ratios: 0.13:1.27:1.31:0.31:0.19:3.94:1.02. Among all the monosaccharides, galactose content is the highest in PSP with (70.89±0.38) mg/g. A positive correlation between the concentration of PSP and the DPPH radical scavenging capacity is confirmed for the hand creams. The DPPH radical scavenging capacity of the hand cream prepared with 10% PSP is several times better than that of PSP-free hand cream. The moisturizing ability of the hand cream is also increased with the increase of PSP concentration. The moisturizing rates of the hand cream prepared with different concentrations of PSP are around 80% within 24 h and 60% within 48 h, while the moisturizing rate of PSP-free hand cream is only 58.17%±1.45% within 24 h and 38.09%±1.56% within 48 h. In the steady-state flow curves and oscillation strain curves of rheological properties, the viscosity of all hand cream samples significantly decreases in relatively low shear rate, whereas the viscosity is low and tends to a fixed value in high shear rate. The PSP added does not change the stability of the hand cream.

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    Mechanism of Citrus reticulata extract in relieving skin sensitivity
    Zhou Lidan,Lu Yina,Liu Qing
    2022, 52 (4):  418-424.  doi: 10.3969/j.issn.1001-1803.2022.04.011
    Abstract ( 362 )   HTML ( 11 )   PDF (1232KB) ( 332 )  

    Citrus reticulata Tangerine) extract (CR) was prepared according to a proprietary process from immature citrus fruit and it was rich in flavonoids and alkaloids. To investigate the mechanism of CR in relieving skin sensitivity through transient receptor potential vanilloid 1 (TRPV1), TRPV1 over-expression cells, prostaglandin receptor 1(EP1) over-expression cells and neuroblast cells were prepared. A comparison between normal cells and TRPV1 over-expression cells showed that, capsaicin (CAP) and phenoxyethanol could increase the expression of interleukin 8, chemokine MCP-1 and prostaglandin E2 (PGE-2) by activating TRPV1 and decrease the migration rate of wound healing. However, the results showed that CR could significantly inhibit the overexpression of cytokines, especially for PGE-2, and could also promote the migration rate of wound healing. Furthermore, the PGE-2-EP1 signaling pathway was studied, and it was found that 0.5% volume fraction of CR could significantly inhibit the activation of luciferase induced by PGE-2 through its receptor EP1. Finally, it was verified on neuroblast cells, and it was found that 0.06%-0.25% volume fraction of CR could inhibit the extracellular Ca2+ influx induced by the activation of TRPV1 caused by CAP and phenoxyethanol, and then inhibit the signal transduction in skin sensitivity or skin irritation, and finally alleviate clinical symptoms such as heat, itching and pain. Therefore, through the control of the activation of TRPV1, CR can inhibit the secretion of nociceptive cytokines and the downstream signal transduction, promote skin barrier repair, and alleviate skin irritation and sensitivity caused by the external stimuli.

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    Reviews
    Study on the application of safety assessment data for toothpastes
    Gong Jingyu,Deng Quanfu,Chen Feng,Dong Haide,Xu Jing,Zhang Min
    2022, 52 (4):  425-430.  doi: 10.3969/j.issn.1001-1803.2022.04.012
    Abstract ( 299 )   HTML ( 20 )   PDF (933KB) ( 316 )  

    Toothpaste safety assessment has been conducted with the principle of industry self-discipline in China. To implement the Cosmetics Supervision and Administration Regulation (CSAR), safety assessment of these products shall become part of the notification dossiers in future. Due to the uneven abilities of safety assessment and the uneven mastery of database, many companies have faced severe challenges when conducting safety assessment. Herein, the applications of domestic and foreign research data in toothpaste product safety assessment were introduced, such as China national standard “General requirements on raw materials of toothpastes”, data from food industry (food additives, condiments, new food raw materials) and traditional Chinese medicine, as well as findings and resources from cosmetic ingredient review (CIR), scientific committee on consumer safety (SCCS), joint FAO/WHO expert committee on food additives (JECFA), etc. The applicability of toxicological test methods for related products in China was also discussed. Based on the current standards, rules, guidelines and assessment data or conclusions, combined with the characteristics of toothpastes, the applications of safety assessment database and toxicological test methods related to toothpastes were summarized, which could provide a useful reference for conducting safety assessment.

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    Research progress of the detection methods for cosmetic risk substances
    Zhou Xinyu,Fan Meimei,Wen Xuehua,Dong Yinmao,Meng Hong,Guo Miaomiao
    2022, 52 (4):  431-437.  doi: 10.3969/j.issn.1001-1803.2022.04.013
    Abstract ( 299 )   HTML ( 20 )   PDF (941KB) ( 346 )  

    Cosmetic risk substances refer to the substances that are brought in by cosmetic raw materials or produced or brought in during the production process, and may cause potential harm to human health. Cosmetics have gradually become indispensable personal care products in people’s daily life. With the continuous expansion of the cosmetics consumer market, the diversified characteristics of cosmetic products, under the influence of fashion trends, make the consumer groups more extensive. The increase in people’s safety awareness and the frequent occurrence of cosmetic safety incidents in recent years have shown that the current situation of cosmetic safety in China is not optimistic. Cosmetics are daily-use chemical industrial products, and they are applied to the surface of human skin for a long time, which are closely related to the health and vitality of users. The safety of cosmetics is important. Cosmetic risk substances are paid special attention to by cosmetic companies and regulatory authorities in cosmetic safety assessment. Herein, the source of cosmetic risk substances was introduced. Combined with the importance of risk assessment and the possible influences of cosmetic risk substances on human health, many cosmetic risk substances such as dioxane, heavy metals, nitrosamines, asbestos, phenol, etc., were listed. The existing testing methods and the relevant testing methods in the “Cosmetics Safety Technical Specifications” were summarized. Moreover, the research progress for cosmetic risk substances in China, EU, US and Japan was also summarized in terms of regulations and policies, risk assessment and detection methods.

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    Analytical methods and testing
    Determination of 2, 4, 6-trichlorophenol, pentachlorophenol and bithionol in soap by salting out phase separation extraction -high performance liquid chromatography
    Zhang Lieyuan,Liu Jieguang,Han Ying,Wan Jianchun,Zhan Chunrui,Wang Wenjun
    2022, 52 (4):  438-443.  doi: 10.3969/j.issn.1001-1803.2022.04.014
    Abstract ( 239 )   HTML ( 11 )   PDF (1249KB) ( 270 )  

    An efficient high performance liquid chromatography analysis method for detecting the content of prohibited preservatives 2, 4, 6-trichlorophenol, pentachlorophenol and bithionol in exported cosmetic soaps was established. There is no literature about the determination of 2, 4, 6-trichlorophenol, pentachlorophenol and bithionol method in soaps. The sample was made into uniform crumbs, dissolved in hot water, mixed with acetonitrile for extraction, and was salted out to obtain the extracting solution. Gradient elution was carried out with methanol-acetonitrile-ammonium acetate as ternary mobile phase. It was at a flow rate of 1.0 mL/min through an Agilent ZORBAX Eclipse XDB-C18 chromatographic column (5 μm, 4.6 mm×250 mm), and the column temperature was 30 ℃. The UV detection wavelength was 300 nm. The external standard method was used for quantification. The experimental results show that the linear correlation coefficients of the three substances are more than 0.999. The limit of detection (LOD) and the limit of quantification (LOQ) of 2, 4, 6-trichlorophenol and pentachlorophenol are 1.5 and 5.0 mg/kg, respectively, and the limit of detection (LOD) and limit of quantification (LOQ)of bithionol is 0.8 and 2.5 mg/kg, respectively. Average recoveries of standard addition at three levels are in the range of 81.8% to 103.0%, with the relative standard deviation (RSD) in the range of 3.88% to 8.57% (n=6). The method is quick, accurate and economical. It is suitable for the quick screening and quantitative analysis of 2, 4, 6-trichlorophenol, pentachlorophenol and bithionol in exported cosmetic soaps. It fills the blank of determination method of the three substance in exported cosmetic soaps, and provides testing technology support for customs supervision of exported cosmetic soaps.

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    Filtered solid phase extraction-UPLC-MS/MS for determination of 35 glucocorticoids in hair-rearing solutions
    Xu Xiaohui,Wang Xiaoqiao,Zhao Bo,Du Ruihu,Zhang Hongyan,Shi Xiaofeng
    2022, 52 (4):  444-450.  doi: 10.3969/j.issn.1001-1803.2022.04.015
    Abstract ( 213 )   HTML ( 4 )   PDF (1044KB) ( 216 )  

    Hair-rearing solutions is a cosmetic product that promotes hair growth, produces new hair and prevents hair loss. More and more people are suffering from hair loss problems in our country. There is a huge profit space in the market of hair growth products at home and abroad, and behind the rising for market profits, the quality problem of hair-rearing solutions often exists. For enhancing the efficacy of hair care products, the illegal drugs are added, which are mainly glucocorticoids. There are many side effects after the use of glucocorticoids, which include obesity, osteoporosis, hyperglycemia, hyperlipidemia, the appearance of acne, hirsutism, atrophic lines, etc. So the medical community at home and abroad takes the use of glucocorticoids extremely seriously. Meanwhile, glucocorticoids have been listed as prohibited substances for cosmetics in statutory standards. In recent years, glucocorticoids are being abused by some manufacturers and beauty salons as ingredients for hair loss prevention and hair growth, which leads to disruption of the hormonal balance and causes various diseases. Currently, there is no literature on determination of glucocorticoids in hair-rearing solutions. In order to assess the glucocorticoids in hair-rearing solutions, a comprehensive analytical method was developed for qualitative and quantitative determination of 35 glucocorticoids in hair-rearing solutions by ultra-performance liquid chromatography coupled with triple quadrupole mass spectrometry (UPLC-MS/MS). The sample was dispersed with saturated sodium chloride and extracted by acetonitrile, then purified with PRiME HLB. The chromatographic separation was performed on an ACQUITY BEH C18 chromatographic column(1.7 μm, 2.1 mm×100 mm), with 0.1% formic acid and 2 mmol/L ammonium acetate of water and 0.1% formic acid of acetonitrile as mobile phases by gradient elution. The multiple reaction monitoring (MRM) acquisition mode was used for detection, and external standard method was used for quantitative detection. Results show that this method exhibits a perfect performance in chromatographic separation. The calibration curves for analytes are of good linearities in concentration ranges of 2-30 ng/mL with the coefficient of determination (R2) no less than 0.99. The limit of detection (LOD, S/N≥3) and quantitation (LOD, S/N≥10) are in the ranges of 0.01-0.65 µg/L and 0.03-2.20 µg/L, respectively. The spiked average recoveries for analytes at their spiked levels are in the range of 62.4%-92.9%, and RSD are 1.7%-5.7%. The method can simultaneously detect 35 glucocorticoids in hair-rearing solutions and can be used to monitor the quality and safety of hair-rearing solutions.

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    Determination of the content of Gardenia jasminoides Ellis from different producing areas by HPLC
    Wu Wentao,Zhao Yulin,Liu Yazhi
    2022, 52 (4):  451-456.  doi: 10.3969/j.issn.1001-1803.2022.04.016
    Abstract ( 223 )   HTML ( 13 )   PDF (1031KB) ( 241 )  

    The contents of the main components of Gardenia, such as geniposide and gardenia yellow pigment, were determined by HPLC method, and the gardenia from different areas were compared. By using a C18 (4.6 mm×250 mm, 5 μm) chromatographic column, the aqueous phase uses 0.2% phosphoric acid solution, the organic phase uses methanol-acetonitrile, the detection wavelength is 254 nm, the elution rate is 1 mL/min, and the column temperature is 30 ℃. The determination of the main components in Gardenia from different origins was carried out below. The experimental results show that the 10 main components of the solution have a good linear relationship, and the average sample recovery rate is 97.3%-103.4%. By comparing the determination results of Gardenia extracts from different origins, it can be seen that the Gardenia extract from Pingyuan County, Jiangxi Province has the highest amount of the main contents. The experimental method used in this paper has certain reliability and can help the medicinal research of Gardenia.

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