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    2022年, 第52卷, 第11期 刊出日期:2022-11-22 上一期    下一期
    基础研究
    低渗透油藏缓释型表面活性剂纳米载体研究
    Study on slow-release surfactant nanocarriers in low-permeability reservoirs
    康万利,王康辉,李哲,吕伟,杨红斌,贾茹雪,何瑛琦
    2022 (11):  1147-1154.  doi: 10.3969/j.issn.1001-1803.2022.11.001
    摘要 ( 1820 )   HTML ( 23 )   PDF(1995KB) ( 235 )  

    为解决低渗透油藏表面活性剂驱吸附严重的问题,以蜂蜡、TX-10和去离子水分别为油相、表面活性剂和水相,采用超声乳化法在高于蜂蜡熔点温度(61 ℃)下制备纳米乳液,进一步降低温度将TX-10固定在油相内部,得到一种缓释型表面活性剂纳米载体。借助紫外可见分光光度计、粒度分析仪、界面张力仪、接触角测量仪等测定了纳米载体的包裹率以及驱油有关性能。结果表明,随着TX-10质量浓度的增加,纳米载体的平均粒径先减小后增加,在5 000 mg/L时粒径最小约105 nm,且对TX-10的包裹率约为90%;在地层温度(65 ℃)下,纳米载体可降低模拟油/水界面张力至3.24×10-2 mN/m,降低表面张力至23.3 mN/m,优于TX-10溶液,并在降低界面张力过程中表现出缓释性;此外,纳米载体可使亲油岩心表面发生润湿反转,与TX-10溶液性能相似,静吸附损失率小于0.1%,较TX-10溶液降低10倍以上;在30和65 ℃下,纳米载体的洗油效率分别是87.7%和92.3%,较TX-10溶液提高约4%。本研究制备的纳米载体可携带表面活性剂在地层孔隙中运移,与原油接触缓慢释放表面活性剂,在保证表面活性剂自身性能的同时具备抗吸附能力,对于低渗透油藏提高采收率表现出较好的应用前景。

    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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    C12-14仲醇乙氧基化物的合成与性能研究
    Synthesis and performance study of C12-14 secondary alcohol ethoxylates
    李映雪,孙永强,周婧洁,孙晋源,梁慧斌,刘瑜琦
    2022 (11):  1155-1161.  doi: 10.3969/j.issn.1001-1803.2022.11.002
    摘要 ( 1220 )   HTML ( 20 )   PDF(1169KB) ( 351 )  

    以KOH、CH3OK为催化剂催化C12-14仲醇乙氧基化反应合成了环氧乙烷加合数为3的仲醇聚氧乙烯醚表面活性剂SAEO3。评价了两种催化剂的催化C12-14仲醇乙氧基化反应活性。系统考察了催化剂的变化对SAEO3性能(包括表面性能、物化性能和应用性能等)的影响。并将实验室合成的SAEO3与市售Secol-30产品的各项性能进行对比。得出的结论如下:相比于KOH催化剂,利用CH3OK催化仲醇乙氧基化反应时,该催化剂反应活性和产物选择性较高。SAEO3与市售Secol-30产品物化性能比较接近,CH3OK催化得到的仲醇醚的浊点高于其他产品。SAEO3的cmc低于市售Secol-30产品。但Secol-30降低表面张力的能力更加优越些,在较低浓度下可将水溶液的表面张力降低至28.25 mN/m。SAEO3产品的应用性能润湿、乳化、泡沫,去污能力均优于Secol-30。该类仲醇聚氧乙烯醚属于低泡表面活性剂,无凝胶相区且去污能力优越,因此可将其应用于浓缩洗涤剂产品中。

    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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    科技讲座
    常用化妆品成型技术(V)——仿生物膜:脂质体
    Common cosmetic preparation technologies (V)Artificial biological membrane: Liposomes
    石晶,冯云,亓玺,徐桂云,范金石
    2022 (11):  1162-1168.  doi: 10.3969/j.issn.1001-1803.2022.11.003
    摘要 ( 1323 )   HTML ( 22 )   PDF(1340KB) ( 404 )  

    脂质体是由磷脂等双亲性物质形成的内部为水相、具有类细胞膜结构的双分子层闭合囊泡,可同时将脂溶性活性物和水溶性活性物分别包封于脂质双层膜及内部的水相中。脂质体作为一种与生物膜结构高度相似,具有良好生物相容性、生物体内可降解、无毒、无免疫原性、副作用低、靶向输送、缓释控释等多种优良特性的一类功效成分载体,已在医药、食品、化妆品等多个行业领域中得到广泛研究和应用。本文介绍了脂质体的组成、结构、分类、理化性质和制备方法,并简析了脂质体剂型的特点及与药品、化妆品应用密切相关的透皮吸收机理,同时对脂质体在医疗、食品、化妆品中的应用情况及未来研发方向做了简要概述。

    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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    开发与应用
    Ca (H2PO42-H3PO4-K2SO4体系两步法制备KH2PO4过程中硫酸钙晶型和形貌调控
    Regulation of crystal form and morphology of gypsum during two-step preparation of KH2PO4 via Ca(H2PO42-H3PO4-K2SO4 system
    叶文财,吴钦,易芸,于文,曹建新
    2022 (11):  1169-1178.  doi: 10.3969/j.issn.1001-1803.2022.11.004
    摘要 ( 2197 )   HTML ( 8 )   PDF(4158KB) ( 278 )  

    在Ca(H2PO42-H3PO4-K2SO4体系中,通过调控较低温度下CaSO4·2H2O结晶和较高温度下CaSO4·2H2O向CaSO4·0.5H2O转晶的两步法晶化反应,制备KH2PO4及副产品α型半水硫酸钙。研究了反应条件对两步晶化过程中CaSO4晶型和形貌、磷钾收率和脱钙率的影响。结果表明,反应温度、反应时间、K2SO4溶液浓度、SO42-过量系数、CaO/P2O5摩尔比和P2O5含量等参数的变化对CaSO4晶型形貌、磷钾收率和脱钙率具有明显影响。一步反应和结晶温度为70 ℃、反应和结晶时间为60 min、二步转晶温度为102 ℃、转晶时间为5.0 h、K2SO4质量分数10%、SO42-过量系数1.2、CaO/P2O5摩尔比0.20、P2O5质量分数25%条件下,滤液钾收率、磷收率和脱钙率分别达98.35%,91.43%和89.74%,制得石膏样品晶型为α-CaSO4·0.5H2O、形貌呈六棱形锥面短柱状、2 h抗折强度和绝干抗压强度分别达5.70 MPa和35.07 Mpa、强度等级达到JC/T 2038-2010《α型高强石膏》α30要求。制得的磷酸二氢钾纯度达80%以上。

    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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    甘油和1,3-丁二醇在D相乳化法制备卸妆油中的应用研究
    Research on the application of glycerin and 1.3-butanediol in the preparation of cleansing oil by D-phase emulsification method
    董蕾蕾, 黄天怿, 蔡屹超, 段国兰, 吴旭, 周千慧, 张冬梅
    2022 (11):  1179-1187.  doi: 10.3969/j.issn.1001-1803.2022.11.005
    摘要 ( 2036 )   HTML ( 35 )   PDF(2798KB) ( 368 )  

    采用D相乳化法制备卸妆油,选择PEG-20甘油三异硬脂酸酯为乳化剂,以甘油或1,3-丁二醇为助乳化剂,选用矿物油、烷烃类、酯类中的10种油脂,系统分析油脂和多元醇在D相乳化过程中对所形成乳液的外观、电导率、微观结构和乳液类型的影响。研究结果表明:按照m (油脂)∶m (乳化剂)∶m (助乳化剂)=6∶3∶1的比例,发现矿物油(7#、10#)、棕榈酸乙基己酯与两种多元醇均可以形成透明的卸妆油体系,而异十六烷仅可以与1,3-丁二醇作用得到相同体系。通过观察乳液外观和电导率变化,发现酯类油脂与甘油的界面张力越大,形成的体系透明度越高,粒子的粒径越小。与甘油相比,1,3-丁二醇可以提升D相乳化过程中微乳液的透明度和粒子的导电能力,更易形成双连续相结构,应用于卸妆油配方体系中。

    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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    利用秀丽线虫评价神经传递抑制肽的祛皱功效研究
    Evaluation of anti-wrinkle effect of neurotransmission inhibitory peptides by Caenorhabditis elegans
    刘涵,郭朝万,陈杰,聂艳峰,胡露,王娟
    2022 (11):  1188-1194.  doi: 10.3969/j.issn.1001-1803.2022.11.006
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    随着化妆品行业迈进高科技发展时期,人们更加注重皮肤的保养,特别是对皮肤纹理平整和皱纹淡化的需求剧增,然而抗皱类化妆品或原料的功效评估存在周期较长、费用较高且无法实现高通量检测的问题。因此,建立可行、有效的替代检测模型实现化妆品原料祛皱功效的快速评价对化妆品开发具有重要意义。作者以秀丽线虫为模式生物,研究几种神经传递抑制类化妆品祛皱多肽对其运动行为和神经递质传导相关酶活性的影响,从而实现化妆品原料祛皱功效的定性定量检测。结果表明,红蝎素、蛇毒肽、芋螺肽以及红蝎素EX(红蝎素和芋螺肽的复配肽)均有一定的阻断神经与肌肉间神经冲动、抵御兴奋刺激条件下线虫神经与肌肉间神经冲动以及显著抑制线虫的运动行为的能力。此外,神经递质传导相关酶活性的数据表明上述神经抑制类多肽是通过刺激钙调神经磷酸酶CaN过表达同时抑制乙酰胆碱酯酶AchE的活力,从而阻断神经与肌肉间神经递质的传递,抑制神经冲动,使肌肉达到放松进而平整皮肤表面、达到祛皱的效果。

    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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    绿原酸通过SIRT6改善UVB诱导的HaCaT炎症反应
    Chlorogenic acid ameliorates UVB-induced HaCaT inflammation through SIRT6
    武思敏,满佳旭,袁梅,高梓琪,王冬雪,张冬英
    2022 (11):  1195-1201.  doi: 10.3969/j.issn.1001-1803.2022.11.007
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    研究绿原酸(CGA)对UVB诱导的HaCaT细胞炎症反应的调节作用及机制。用CGA干预UVB处理的HaCaT细胞,结晶紫染色法检测CGA对UVB损伤HaCaT细胞的保护作用。通过酶联免疫吸附法检测细胞内TNF-α含量的变化,ABTS、DPPH、FRAP法检测CGA在细胞内外的抗氧化能力,丙二醛试剂盒法检测细胞中MDA含量,CM-H2DCFDA染色法检测细胞内总活性氧的变化,Western Blot法检测SIRT6、TNF-α、P-AKT、P-AMPK、AMPK、β-Tubulin蛋白的相对表达量。结晶紫染色表明100和150 μmol/L CGA对于21.6 mJ/cm2 UVB处理的HaCaT细胞具有保护作用。酶联免疫吸附法证明了CGA处理能够显著降低TNF-α的表达(P<0.01)。CGA在细胞内外均具备良好的自由基清除能力,并且能够有效降低UVB诱导的MDA和ROS的产生。CGA可以显著抑制由UVB引起的SIRT6表达上调,从而降低AKT的磷酸化水平,活化AMPK进而降低TNF-α的表达,缓解细胞的炎症反应。CGA可以抑制SIRT6的表达进而降低UVB诱导的HaCaT的炎症反应,并且降低UVB造成的细胞的氧化应激,具有很强的抗皮肤光老化活性。

    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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    7种植物精油对糠秕马拉色菌抑制效果比较及樟树精油抑菌作用研究
    Inhibitory effects of seven plant essential oils against Malassezia furfur and the antimicrobial mechanism of Cinnamomum camphora essential oil
    何园,李自强,孙伟杰,马淑梅,刘莉
    2022 (11):  1202-1207.  doi: 10.3969/j.issn.1001-1803.2022.11.008
    摘要 ( 465 )   HTML ( 20 )   PDF(2048KB) ( 308 )  

    通过比较7种精油的抗糠秕马拉色菌活性,筛选作用效果最佳的植物精油并进一步分析其对糠秕马拉色菌的抑制作用。采用K-B纸片扩散法和微量肉汤稀释法筛选抑菌作用效果最佳的植物精油,同时利用气相色谱-质谱联用仪(GC-MS)对效果最佳的植物精油的挥发性成分进行鉴定,进一步对其主要化学成分与抗糠秕马拉色菌活性进行相关性分析,然后利用扫描电镜(SEM)和透射电镜(TEM)观察糠秕马拉色菌形态变化,最后采用流式细胞术检测其对糠秕马拉色菌细胞凋亡的影响。结果表明樟树精油抗糠秕马拉色菌的活性强于其他6种精油;GC-MS共鉴定出14个化学成分且抗糠秕马拉色菌活性来源于3-蒈烯、松油烯-4-醇、α-松油烯、异松油烯;SEM显示樟树精油使糠秕马拉色菌细胞轻度损伤,局部细胞膜凹陷;TEM显示樟树精油使糠秕马拉色菌质壁分离,胞内基质变淡;樟树精油会使糠秕马拉色菌凋亡明显增加。综上,樟树精油对糠秕马拉色菌作用效果显著,其可通过破坏菌体细胞壁与细胞膜,实现其抑菌效果。

    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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    短梗五加多糖的结构解析及抗氧化活性分析
    Structural analysis and hypoglycemic activity analysis of polysaccharides from Acanthopanax sessiliflorus
    杨永鹏,修玉武,黄维芝
    2022 (11):  1208-1213.  doi: 10.3969/j.issn.1001-1803.2022.11.009
    摘要 ( 155 )   HTML ( 7 )   PDF(1220KB) ( 172 )  

    对短梗五加中的多糖组分进行分离纯化,通过实验解析组分结构,并对其抗氧化活性进行分析。从短梗五加茎中分离纯化短梗五加多糖,通过高效液相色谱法、气相色谱-质谱分析、傅里叶变换红外光谱和紫外-可见光光谱法、1H NMR和13C NMR等对其组成结构特征进行研究和分析,并考察了短梗五加多糖对1,2-二苦基-2-三硝基苯亚肼(DPPH)、2,2-联氮-二(3-乙基-苯并噻唑-6-磺酸)二铵盐(ABTS)的抗氧化能力和铁离子还原能力。实验结果表明,短梗五加多糖由甘露糖、葡萄糖、半乳糖、阿拉伯糖组成,结构主要由吡喃糖环状构成,可以有效清除DPPH、ABTS阳离子自由基,还原铁离子。证明短梗五加多糖具有较好的抗氧化生物活性。

    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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    密泡牙膏的试验研究
    Experimental study on dense foam toothpaste
    易瑞,徐春生
    2022 (11):  1214-1220.  doi: 10.3969/j.issn.1001-1803.2022.11.010
    摘要 ( 229 )   HTML ( 10 )   PDF(1774KB) ( 265 )  

    研究了烷基糖苷(APG)分别与十二烷基硫酸钠(K12)、月桂酰肌氨酸钠(LS-30)、椰油酰谷氨酸钠、甲基椰油酰基牛磺酸钠、生物糖脂和辛酰/癸酰胺丙基甜菜碱六种发泡剂按1∶1比例复配时在牙膏常用比例的三元溶液中的pH值、泡沫量和泡沫稳定性,并以此为基础自制了碳酸钙型牙膏和二氧化硅型牙膏,测量了自制牙膏的pH值、泡沫量和发泡速度,再分别与以K12作为发泡剂的牙膏对比做了密泡试验。另外,还测试了几款市售二氧化硅型高泡牙膏的泡沫量并与自制二氧化硅型牙膏进行对比。通过以上几种方法对以APG为主、复配其他发泡剂的自制牙膏所产生的泡沫性能进行全面评价,结果表明,APG分别复配K12、LS-30、甲基椰油酰基牛磺酸钠、生物糖脂后的碳酸钙型及二氧化硅型牙膏均泡沫量增加、泡沫稳定性提高、发泡速度更快,且牙膏pH在其他成分的缓冲下均处于理想的范围内。

    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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    专论与综述
    我国化妆品原料安全信息库的建立及其应用展望
    Establishment and prospects of the database for safety information on cosmetic ingredients in China
    苏哲,胡康,王钢力,路勇
    2022 (11):  1221-1228.  doi: 10.3969/j.issn.1001-1803.2022.11.011
    摘要 ( 1347 )   HTML ( 21 )   PDF(1003KB) ( 262 )  

    在新修订的《化妆品监督管理条例》背景下,国家药监局构建了全新的化妆品法规和技术体系,加强了化妆品原料管理和安全评估,并提出化妆品原料安全信息报送相关要求。中检院结合法规要求和监管实际需求,围绕化妆品原料的精细化管理开展一系列相关研究,包括原料分类和关键特征、原料基本信息、原料鉴别和特征性指标、风险信息和控制指标、安全信息使用等,并据此建设“化妆品原料安全信息登记平台”,用于化妆品原料安全信息的规范化填报和管理。通过对化妆品原料安全信息的收集、利用和分析,同时对化妆品法规标准相关数据库不断研究整合,将在我国逐步构建起科学高效的“化妆品原料安全信息库”,在化妆品技术监管工作中提供有力的大数据支撑,不断提高我国的化妆品监管和安全性评价水平。

    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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    视觉文化融入与心理驱动因素结合在化妆品外包装设计中的应用
    Application of visual culture integration and psychological driving factors in cosmetic packaging design
    郑蔚
    2022 (11):  1229-1235.  doi: 10.3969/j.issn.1001-1803.2022.11.012
    摘要 ( 169 )   HTML ( 5 )   PDF(1154KB) ( 165 )  

    优质的化妆品外观包装设计可有效增加消费者品牌信任度,提升化妆品销量和品牌知名度。研究将视觉文化与心理驱动因素相结合,融入到化妆品外观包装设计中,从社会、消费观念和生产者利润空间三方面,研究视觉文化在化妆品外观包装设计中的体现;另外,从动机、消费者需求驱动、实用性驱动和体验驱动三方面,研究心理驱动因素在化妆品外观包装视觉设计中体现。针对以上研究所得结果,提出化妆品外观包装设计的新策略,以视觉文化设计引导消费者心理驱动作为导向,从多个心理驱动角度进行视觉文化设计,吸引消费者注意力和兴趣、激发消费者购买欲望、促成消费者购买行为,为化妆品包装设计提供新思路。

    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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    分析与检测
    高效液相色谱法检测发酵液中四氢嘧啶及羟基四氢嘧啶
    Determination of ectoine and hydroxyectoine in fermentation broth by high performance liquid chromatography
    刘紫寒,郭秋爽,周超,孙杨,李华,刘宇鹏
    2022 (11):  1236-1240.  doi: 10.3969/j.issn.1001-1803.2022.11.013
    摘要 ( 459 )   HTML ( 18 )   PDF(1161KB) ( 377 )  

    为实现发酵液样品中四氢嘧啶和羟基四氢嘧啶的分离检测,使用高效液相色谱(HPLC)技术建立一种测定中度嗜盐菌发酵液中四氢嘧啶及羟基四氢嘧啶含量的方法。使用乙醇抽提法提取样品,采用VertexTM NH2 (4.6×250 mm,5 μm)液相色谱柱对中度嗜盐菌发酵液中四氢嘧啶及四氢嘧啶进行了分析,选用紫外(UV)检测器,对比不同检测条件。通过色谱条件优化,选定了70%乙腈作为流动相,柱温30 ℃,检测波长210 nm,流速0.8 mL/min。发酵液样品中四氢嘧啶和羟基四氢嘧啶在各自范围内线性关系良好,两种样品的平均回收率在99.2%~102%,精密度偏差在1%~2%范围内,检出限为1.5 μg/mL,定量限为5 μg/mL,分离度为1.70。该方法检测范围大,具有较好的重复性、分离度及稳定性,适用于发酵液中四氢嘧啶及羟基四氢嘧啶的分离检测。

    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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    HPLC法检测婴幼儿与成人护肤品中防腐剂添加情况的研究
    Study on the detection of preservatives in infant and adult skin care products by HPLC
    刘慧,李莉,刘婷媛,徐勤科,孙莺,郭朝晖
    2022 (11):  1241-1247.  doi: 10.3969/j.issn.1001-1803.2022.11.014
    摘要 ( 171 )   HTML ( 9 )   PDF(1165KB) ( 192 )  

    为了探究婴幼儿和成人护肤品中防腐剂添加情况,以期为婴幼儿和成人护肤品中防腐剂的安全监控与质量研究积累科学数据。以市售的140批护肤类产品为研究对象,基于国家药品监督管理局2021年第17号通告为检验依据对样品中防腐剂进行检测,将检测结果统计分析。结果表明:线性相关系数均大于等于0.9969,加标回收率为91%~104%,RSD小于5.0%。产自广东省和上海市的样本较多,未出现超限度情况,未检出禁用组分。苯氧乙醇和尼泊金酯类的甲丙酯使用频率较高;苯氧乙醇在婴幼儿护肤品中使用率较高;甲丙酯均在驻留类产品中普遍复合添加,且成人护肤品中的使用率高。婴幼儿护肤品中单批样品检出1~3种组分最多共有54批,成人护肤品中单批样品检出1~3种组分最多共有62批。婴幼儿护肤品防腐剂使用量0~2.3%明显高于成人护肤品使用量。结论:该试验下婴幼儿与成人护肤类产品中多以添加1~3种防腐剂成为防腐主流,且以苯氧乙醇和尼泊金酯类的甲丙酯为主要组分。

    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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    高效液相色谱法测定牙膏中防腐剂含量
    Determination of preservatives in toothpaste by high performance liquid chromatography
    张晓萍,王世芳
    2022 (11):  1248-1253.  doi: 10.3969/j.issn.1001-1803.2022.11.015
    摘要 ( 190 )   HTML ( 9 )   PDF(1154KB) ( 176 )  

    为管理限制牙膏中防腐剂的种类与用量,提升牙膏质量,研究利用高效液相色谱法测定牙膏中防腐剂的含量。用对羟基苯甲酸甲酯、对羟基苯甲酸乙酯以及苯甲酸等5种试剂制备防腐剂混合标准溶液,利用乙腈等溶液处理牙膏样本,采用高效液相色谱仪,以磷酸二氢钠溶液、甲醇与乙腈混合溶液为流动相,在柱温为室温,进样量为5 μL,流速为1.5 mL/min的条件下测定混合标准溶液与牙膏样本,并根据混合标准溶液色谱峰的保留时间与面积绘制标准曲线。结果显示:流动相内磷酸二氢钠溶液、甲醇与乙腈体积比为55∶25∶20的条件下,混合标准溶液的分离度最高;各类防腐剂回收率范围为88.68%~99.61%之间,相对标准偏差范围为0.39%~2.44%之间;重复性测试结果满足实际应用需求。

    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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    气相色谱质谱法测定化妆品中薄荷醇和薄荷醇乳酸酯
    Determination of menthol and menthyl lactate in cosmetics by GC-MS
    熊智,施佳佳,何泉泉
    2022 (11):  1254-1258.  doi: 10.3969/j.issn.1001-1803.2022.11.016
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    对比了不同构型薄荷醇在定性、定量分析方面的差异性,建立了气相色谱质谱法同时测定化妆品中薄荷醇和薄荷醇乳酸酯,样品经甲醇超声提取,以VF-WAXms(30 m×0.25 mm×0.25 μm)色谱柱分离,选择特征离子监测(SIM)扫描模式测定,外标法定量。结果表明,在此实验条件下,不同构型的薄荷醇在响应、保留时间和全扫描质谱图等方面无明显差异。薄荷醇和薄荷醇乳酸酯在0.1~100 mg/L范围内线性良好,相关系数均大于0.999,检出质量浓度分别为0.009和0.002 mg/L,检出限分别为0.9和0.2 mg/kg,定量质量浓度分别为0.027和0.006 mg/L,定量限分别为2.7和0.6 mg/kg,加标回收率为96.3%~100.7%,相对标准偏差为1.9%~3.5%。该方法操作简便,灵敏度高,准确度高,适用于化妆品中薄荷醇和薄荷醇乳酸酯的检测。

    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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