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欢迎访问《日用化学工业(中英文)》,今天是

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    2021年, 第51卷, 第10期 刊出日期:2021-10-22 上一期    下一期
    基础研究
    液滴模板法构建疏水杂化囊用于包封SOD酶研究
    Preparation of the hydrophobic hybrid capsule via droplet template method for encapsulating SOD
    邓宁君,唐启明,洪美莹,孙梦梦,郭婷,孟涛
    2021 (10):  925-931.  doi: 10.3969/j.issn.1001-1803.2021.10.001
    摘要 ( 259 )   HTML ( 44 )   PDF(1481KB) ( 498 )  

    针对化妆品中生物活性分子保存稳定性问题,通过液滴模板法制备包封超氧化物歧化酶(SOD)的碳酸钙@海藻酸钙(CaCO3@Ca-Alg)杂化囊,再疏水改性壁层来阻止水分子进入,从而提高了包封物的保存稳定性。实验结果表明:该包封SOD的疏水杂化囊具有粒径均一、单分散性良好的优点;随着改性时间的延长,杂化囊疏水性随之提高,当改性时间超过4 h后,杂化囊疏水性保持稳定;杂化囊固定SOD的相对酶活明显高于单纯Ca-Alg囊(最大差值达到了300%);游离SOD在去离子水中保存4 d后完全失活,而包封SOD的疏水杂化囊保存7 d后仍能维持95%以上的相对酶活。

    To solve the problems in the storage stability of bioactive molecules in cosmetics, the CaCO3@Ca-Alg hybrid capsule with encapsulated superoxide dismutase (SOD) was prepared by droplet template method. Combined with the hydrophobic modification of the shell, the hydrophobic layer could prevent the infiltration of water molecules, thus improving the storage stability of the encapsulated substance. The results show that the SOD loaded hydrophobic hybrid capsule possesses uniform particle size and good monodispersity. The hydrophobicity of the hybrid capsule is improved with the increase of modification time. When the modification time is over 4 h, the hydrophobicity of the hybrid capsule remains stable. The relative enzyme activity of SOD encapsulated by this hybrid capsule is significantly higher than that of simple Ca-Alg capsule (the maximum difference can reach 300%). The hydrophobic hybrid capsule can significantly improve the storage stability of SOD which will maintain more than 95% of the relative activity within 7 days.

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    餐厨废弃油脂磺酸盐二元复合驱油效果评价
    Evaluation of enhanced oil recovery of the binary composite flooding system based on the sulfonate of kitchen waste oil and polyacrylamide
    王奇浩,郭海燕,王玉怡,黄小荷,张亚,龙运前
    2021 (10):  932-938.  doi: 10.3969/j.issn.1001-1803.2021.10.002
    摘要 ( 192 )   HTML ( 8 )   PDF(1516KB) ( 270 )  

    经磺化反应制备了餐厨废弃油脂磺酸盐(KWOS),通过降低油水间界面张力性能、热稳定性能、抗钙镁离子性能和吸附损耗性能实验评价了KWOS溶液与原油间界面张力的适应性能。配制KWOS和聚丙烯酰胺的二元复合体系开展驱油实验,分析岩心渗透率和KWOS质量分数对该体系驱油效果的影响。结果表明:随着KWOS质量分数增加,油水间的界面张力逐渐降低,当质量分数达到0.175%时,油水界面张力即可降至10-3 mN/m数量级。KWOS溶液与原油间的界面张力随热稳定时间增长、钙镁离子总质量浓度增大和吸附损耗有所增加,但仍能够维持在10-3 mN/m数量级。随着岩心渗透率降低和KWOS质量分数增加,二元复合体系提高原油采收率均呈现先增加后降低的变化趋势,当岩心渗透率为0.421 μm 2、KWOS质量分数为0.3%时,二元复合体系提高的原油采收率最高。

    The salt of sulfonated kitchen waste oil (KWOS) was synthesized by sulfonation reaction. The interfacial performance between the KWOS solution and the crude oil was evaluated by measurement of interfacial tension, thermal stability, calcium and magnesium ion resistance and adsorption loss. The binary composite systems of polyacrylamide and KWOS were prepared to carry out oil displacement experiments at different permeabilities of core and various mass fraction of KWOS. The influences of core permeability and mass fraction of KWOS on the oil displacement were investigated. The results show that the interfacial tension between oil and water is gradually decreased with the increase of mass fraction of KWOS. When the mass fraction of KWOS reaches 0.175%, the interfacial tension between oil and water can be reduced to the order of magnitude of 10-3 mN/m. The interfacial tension between KWOS solution and crude oil is increased with the increase in thermal stability time, the total mass concentration of calcium and magnesium ions and the adsorption loss, but it can be still maintained in the order of 10-3 mN/m, indicative of a favorable adaptability to oil reservoir. With the decrease of core permeability and the increase of mass fraction of KWOS, the enhanced oil recovery of binary composite system first increases and then decreases. When the core permeability is 0.421 μm 2 and the mass fraction of KWOS is 0.3%, the binary composite system shows the highest enhanced oil recovery, illustrating that there are the best conditions for the binary composite system of polyacrylamide and KWOS in enhanced oil recovery.

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    科技讲座
    化妆品乳液及乳化新技术(Ⅴ)——脂质体包载技术在经皮输送中的应用
    Cosmetic emulsions and new technologies of emulsification (Ⅴ) Application of liposomes entrapment technology in transdermal delivery
    张雅琪,梁蓉,杨成
    2021 (10):  939-948.  doi: 10.3969/j.issn.1001-1803.2021.10.003
    摘要 ( 745 )   HTML ( 26 )   PDF(2037KB) ( 618 )  

    化妆品中所添加的活性成分往往存在光、热稳定性差,溶解性差等原因,需通过包载技术提高其生物利用度。在各种包载体系中,脂质体由于结构与人体皮肤细胞相似,且具有良好的生物相容性,是一种有效的包载方法。然而传统脂质体由于稳定性、可变形性差等原因难以通过皮肤屏障,达到促渗效果。如今,通过改变传统脂质体磷脂双层膜的结构获得了各种新型脂质体,如醇质体、类脂质体、传递体、磷脂复合物、甘油体等,新型脂质体由于稳定性良好、具有可变形性、可改变角质层脂质结构等特点,能够改善药物经皮输送效果。文章综述了几种新型脂质体,并对其透皮效果进行分析,旨在为化妆品包载领域提供借鉴和思路。

    The bioavailability of some active ingredients in cosmetics needs to be improved by nanoencapsulation technology due to their poor light/thermal stability and poor solubility. Among various encapsulation systems, liposomes are effective encapsulation method because of their similar structure to human skin cells and good biocompatibility. However, traditional liposomes are difficult to pass through the skin barrier due to their poor stability and deformability, it’s difficult to achieve the effect of promoting permeability. Nowadays, various new liposomes have been obtained by changing the structure of traditional liposomes’ phospholipid bilayer, such as ethosomes, niosomes, transferosomes, phytosomes, glycerosomes, etc. The effect of drug transdermal delivery has been improved by these new liposomes due to their good stability, deformability and the ability to change the lipid structure of stratum corneum. Herein, several new liposomes have been reviewed and their transdermal effects have been analyzed to provide reference and ideas for the field of cosmetic encapsulation.

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    开发与应用
    神经酰胺纳米乳液的制备及透皮性能研究
    Study on the preparation and transdermal performance of the ceramide nanoemulsion
    王玙璇,梁蓉,骆晔媛
    2021 (10):  949-955.  doi: 10.3969/j.issn.1001-1803.2021.10.004
    摘要 ( 550 )   HTML ( 23 )   PDF(1741KB) ( 430 )  

    为了提高神经酰胺的应用稳定性和生物利用率,采用高压均质法制备了神经酰胺(Ceramide III,Cer3)纳米乳液,研究了卵磷脂用量、甘油与水质量比、均质压力、循环次数及植物鞘氨醇添加量对乳液粒径及稳定性的影响,发现当卵磷脂质量分数为4%,甘油与水质量比为7:1,均质压力为90 MPa,循环9次,植物鞘氨醇质量分数为1.5%时,载体在各温度下具有良好的储藏稳定性;此时载体呈凝胶状并携带正电,Zeta电位为36.67 mV,粒径为200 nm左右,添加植物鞘氨醇显著提高了载体的高温稳定性,奥氏熟化速率由6.06降至1.53,并且由于植物鞘氨醇的添加,Cer3透皮含量由3.02 μg/cm 2增至7.12 μg/cm 2,透皮性能得到显著提高。

    Ceramide is an important lipid in the stratum corneum of skin and plays an indispensable role in maintaining the normal physiological functions of skin. The skin contains the most abundant types of ceramides and there are currently 15 types of ceramides that have been detected. And among them, ceramide3 (Cer3) has the highest content in the skin and is an essential ingredient for regulating skin barrier function. However, Cer3 is very easy to crystallize when directly applied and thus it needs a carrier to improve its stability during application. Therefore, to improve the stability and bioavailability of Cer3, Cer3 nanoemulsions were prepared by high-pressure homogenization method. The effects of the amount of lecithin, the mass ratio of glycerol to water, the homogenization pressure, the number of cycles and the amount of phytosphingosine on the particle size and stability of the emulsions were studied. It is found that when the mass fraction of lecithin is 4%, the mass ratio of glycerol to water is 7:1, the average pressure is 90 MPa and the number of cycles is 9, the emulsion has good stability. Furthermore, phytosphingosine was added to the system to improve the storage stability of Cer3 nanoemulsion at high temperature. The results show that when the mass fraction of phytosphingosine is 1.5%, the Ostwald ripening rate of Cer3 nanoemulsion is decreased from 6.06 to 1.53 and the Cer3 nanoemulsion is gel-like at this time. It is found that the nanoemulsion particles are spherical and have a particle size of approximately 200 nm as observed by TEM. The results of Zeta potential show that the Cer3 nanoemulsion carries a positive charge and the potential is 36.67 mV. The transdermal performance of the Cer3 nanoemulsions with different mass fractions of phytosphingosine was also studied. It is found that the transdermal content of Cer3 is closely related to the potential value of the Cer3 nanoemulsion. When the mass fraction of phytosphingosine is 1.5%, the transdermal content of Cer3 is increased from 3.02 μg/cm 2 to 7.12 μg/cm 2, indicating that the addition of phytosphingosine can effectively improve the transdermal performance of Cer3.

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    脂肪醇聚醚类乳化剂对低粘乳液制备的影响
    Effects of fatty alcohol polyether emulsifiers on the preparation of low-viscosity emulsions
    李喜连,胡璠,陈明华
    2021 (10):  956-962.  doi: 10.3969/j.issn.1001-1803.2021.10.005
    摘要 ( 338 )   HTML ( 21 )   PDF(1646KB) ( 429 )  

    研究乳化剂对低粘乳液制备的影响,从而筛选出适合制备低粘乳液的乳化剂,并通过流变性能对其稳定性进行了初步考察。实验结果表明:鲸蜡硬脂醇聚醚类乳化剂比较适合制备低粘乳液;对于水包油类型乳化剂,相同的亲脂性基团下,亲水基越短屈服应力越高,同时离心稳定性越好。鲸蜡硬脂醇聚醚类乳化剂在配方中单用时存在一个较佳用量,在该用量下与低HLB值非离子乳化剂复配使用后乳液屈服应力明显提高,同时粒径更小。因为配方体系只有乳化剂变化,屈服应力提高很有可能是因为复配乳化剂导致更高的界面膜强度所致。

    The effects of emulsifiers on the preparation of low-viscosity emulsions were studied. The long-term thermal stability of low-viscosity emulsions was monitored by investigating their rheological properties. The results show that cetearyl alcohol polyether emulsifier is suitable for preparing low-viscosity emulsions. For oil-in-water emulsifiers, given the same lipophilic group, the shorter the EO chain length, the better the yield stress and the centrifugal stability of the resulting emulsion. There is an optimal amount for cetearyl alcohol polyether emulsifier when it is solely used as the emulsifier. Its emulsifying property is good. The yield stress of the low-viscosity emulsion is significantly higher when cetearyl alcohol polyether emulsifier is combined with a low-HLB nonionic emulsifier, and the resulting particle size is smaller. It is highly likely due to the stronger interfacial film strength in the presence of two emulsifiers, because the emulsifier is the only variable in the studied emulsions.

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    二醇型人参皂苷W/O纳米乳的制备及其抗皮肤衰老机制研究
    Preparation of diol-type ginsenoside W/O nanoemulsion and research on anti-aging mechanism of skin
    武子超,叶超,朴明贯
    2021 (10):  963-968.  doi: 10.3969/j.issn.1001-1803.2021.10.006
    摘要 ( 390 )   HTML ( 14 )   PDF(1257KB) ( 320 )  

    制备二醇型人参皂苷W/O纳米乳,研究其抗皮肤衰老机制。根据伪三元相图形成的纳米乳区和二醇型人参皂苷的溶解性,筛选二醇型人参皂苷纳米乳的处方;测定纳米乳的形态、粒径分布、载药量及稳定性。采用Franz扩散池研究纳米乳的体外透皮特性,HE染色法考察雄性小鼠局部给药对皮肤微观结构的影响,并考察纳米乳的抗皮肤衰老功效。二醇型人参皂苷W/O纳米乳的最佳处方为棕榈酸异丙酯(油相)、司盘80(乳化剂)、1,2-丙二醇(助乳化剂)、Km值=2、油相与混合乳化剂比例为7.5∶2.5;制得的纳米乳外观圆整、均匀,平均粒径为17 nm,粒径分布系数为0.064,二醇型人参皂苷含量为4.2 mg/mL,且物理稳定性良好。体外透皮实验结果表明,给药12 h后二醇型人参皂苷纳米乳的累计透过量为1.640 7 mg/cm2,皮肤滞留量为0.018 4 mg/cm2,分别为二醇型水溶液的2.832 2倍和1.179 5倍;HE染色实验发现,使用人参皂苷纳米乳后结构基本完整,无病理学病变,真皮胶原纤维致密丰富,多排列成束。动物实验结果表明,二醇型人参皂苷纳米乳高、中、低剂量组的羟脯胺酸、Ⅰ型胶原、Ⅲ型胶原、基质金属蛋白酶抑制剂1(TIMP-1)、基质金属蛋白酶抑制剂2(TIMP-2)含量均显著大于空白组和二醇型人参皂苷水溶液组,基质金属蛋白酶1(MMP-1)含量显著小于空白组和二醇型人参皂苷水溶液组。制备的人参皂苷纳米乳稳定性好,透皮性能优良,能通过抑制皮肤内胶原蛋白分解,提高皮肤中胶原蛋白含量达到抗皮肤衰老功效。

    The diol-type ginsenoside W/O nanoemulsion was prepared and its anti-aging mechanism of skin was studied. According to the solubility of the diol-type ginsenoside and the pseudo-ternary phase diagram, we investigated the nanoemulsion prescription, and determined the nanoemulsion morphology, particle size distribution, drug loading and stability. The Franz diffusion cell was used to study the in vitro transdermal properties of the nanoemulsion, and the effect of local administration of the nanoemulsion on male mice skin microstructure was investigated by HE staining method. And the anti-aging effects of nanoemulsion was investigated as well. The best prescription for diol-type ginsenoside W/O nanoemulsion is isopropyl palmitate as oil phase, Span 80 as emulsifier, 1, 2-propylene glycol as co-emulsifier, and Km value=2. The ratio of oil phase to mixed emulsifier is 7.5∶2.5. The nanoemulsion has a round and uniform appearance, the average particle size is 17 nm, the particle size distribution value is 0.064, and the glycol-type ginsenoside content is 4.2 mg/mL. The physical stability is good. The results of in vitro transdermal experiments show that the cumulative permeation of the ginsenoside nanoemulsion is 1.640 7 mg/cm 2 after 12 h of transdermal administration, which is 2.832 2 times that of the cumulative permeation of 12 h in aqueous solution. The skin retention is 0.018 4 mg/cm2, which is 1.179 5 times that of the skin retention of the aqueous solution. The HE staining experiment is found that the structure of the epidermal structure is basically intact without pathological changes after using the ginsenoside nanoemulsion. The dermal collagen fibers are dense and abundant, mostly arrange in bundles. The results of animal experiments show that hydroxyproline, type I collagen, type III collagen, matrix metalloproteinase inhibitor 1 (TIMP-1), and matrix metalloproteinase inhibitor 2 (TIMP-2) content are significantly higher than the blank group and the ginsenoside aqueous solution group, and the contents of matrix metalloproteinase 1 (MMP-1) are significantly lower than those in the blank group and the aqueous solution group. The prepared ginsenoside nanoemulsion has good stability and excellent transdermal performance, and can achieve anti-aging effects by inhibiting the decomposition of collagen and increasing the collagen content in the skin.

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    β-环糊精固化单宁复合微球制备及吸附性能研究
    Study on the preparation and adsorption properties of β-cyclodextrin/tannin composite microspheres
    金绍娣,顾东雅,石智超
    2021 (10):  969-974.  doi: 10.3969/j.issn.1001-1803.2021.10.007
    摘要 ( 233 )   HTML ( 6 )   PDF(1383KB) ( 276 )  

    β-环糊精、单宁为单体,环氧氯丙烷为交联剂,反相悬浮交联制备β-环糊精/单宁复合微球。通过红外光谱法、X射线衍射法对微球进行表征,证明单宁成功固定在β-环糊精上。以阳离子染料亚甲基蓝为有机吸附质模型,考察了染料初始溶液pH、初始溶液质量浓度对微球吸附性能的影响。吸附性能实验表明,pH在中性条件下,β-环糊精空腔与单宁酚羟基协同作用,有利于提高微球与亚甲基蓝之间的静电吸附能力,吸附率为80.31%;当亚甲基蓝初始浓度增大至1 000 mg/L时,网络中的空隙被填充,吸附位点趋于饱和,吸附量最大达到630.41 mg/g。β-环糊精/单宁复合微球具有较好的重复使用性能,大大提高了2种单体在工业废水吸附领域的应用价值。

    The β-cyclodextrin/tannin composite microspheres (β-CD/TA) were prepared by reverse suspension crosslinking polymerization, using β-cyclodextrin and tannin as monomers, and epichlorohydrin as a crosslinker. The microspheres were characterized by infrared spectroscopy and X-ray diffraction, which proved that tannin was successfully immobilized on β-cyclodextrin. Taking methylene blue (a cationic dye) as the model organic adsorbent, the effects of the pH and mass concentration of the initial solution of the dye on the adsorption performance of the microspheres were investigated. The adsorption experiment showed that the synergistic action between β-cyclodextrin cavity and tannic hydroxyl group was beneficial to improve the electrostatic adsorption between microspheres and methylene blue under neutral pH conditions, and the adsorption rate was 80.31%. When the initial concentration of methylene blue was increased to 1 000 mg/L, the gaps in the network were filled, the adsorption sites tended to be saturated, and the maximum adsorption capacity reached 630.41 mg/g. The β-cyclodextrin/tannin composite microspheres have good reuse performance, which greatly improves the application value of the two monomers in the field of industrial wastewater adsorption.

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    市售无添加防腐剂化妆品防腐体系效能评价
    Evaluation of preservation for preservative-free cosmetics
    李增婷,吕鑫,李倩,曹乾超,崔学文
    2021 (10):  975-980.  doi: 10.3969/j.issn.1001-1803.2021.10.008
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    通过中和剂验证、防腐挑战等试验对市售无添加防腐剂化妆品的防腐体系进行效能评价。采集无防腐剂的化妆品15批次,按《化妆品安全技术规范》(2015年版)(以下简称《规范》)进行菌落总数、霉菌和酵母菌以及pH值测定,参照GB 5009.238—2016《食品安全国家标准食品水分活度的测定》测定水活度,参考国外相关标准进行防腐挑战试验。菌落总数、霉菌和酵母菌的结果均符合《规范》要求。中和剂验证试验有3批(20%)需要替换中和剂或进一步稀释。防腐挑战试验中有14批细菌7天可下降大于99.9%,9批霉菌和酵母菌7天可下降大于90%。9批(60%)样品符合CTFA和AOAC非眼用化妆品的要求。样品普遍为弱酸性或中性,pH值最高9.73,最低4.68;水活度值集中在0.850~1.000,最低为0.643。综合结果表明:按《规范》进行化妆品微生物检验漏检风险较大,部分无添加防腐剂化妆品的防腐体系可能存在安全隐患;中和剂验证及防腐挑战试验亟需加入我国标准体系。

    The preservative performance of preservative-free cosmetics in the market was evaluated by neutralizer verification and preservative challenge testing. 15 batches of cosmetics without preservatives were collected. Total Aerobic Microbial Count (TAMC), Total Molds and Yeasts Count (TMYC) and pH value were determined according to “Safety and Technical Standards for Cosmetics” (2015 Edition)(hereinafter referred to as the Standards). Water activity was determined according to GB 5009.238—2016 “National Food Safety Standard Determination of Water Activity of Food”. Preservative challenge testing was carried out according to the methods of relevant foreign standards. The results of TAMC and TMYC meet the requirements of the Standards. The results of neutralizer verification show that 3 batches (20%) need neutralizer to be replaced or further diluted. The results of preservative challenge testing show that, bacteria of 14 batches decrease by more than 99.9% in 7 days, and molds and yeasts of 9 batches decrease by more than 90% in 7 days. Only 9 batches (60%) of the samples meet the requirements of non-eye cosmetics of CTFA and AOAC. Samples are generally weakly acidic or neutral, with the highest pH value of 9.73 and the lowest of 4.68. The water activity of most samples is in the range of 0.850-1.000, except for the ones with the low values of 0.643 and 0.751. It is shown that, in microbiological determination, the risk of missing rate will be high according to the methods of the Standards, and some preservative-free cosmetics may have potential safety hazards; it is urgent to introduce the neutralizer verification and preservative challenge testing to the national standards of microbiological test for cosmetics.

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    丹参发酵液的体外抗氧化和美白功效评价
    Evaluation of anti-oxidation and whitening efficacy of salvia miltiorrhiza fermentation broth in vitro
    莫秋婷,李萌,王冬冬,张佳婵,王昌涛,赵丹
    2021 (10):  981-989.  doi: 10.3969/j.issn.1001-1803.2021.10.009
    摘要 ( 356 )   HTML ( 18 )   PDF(1804KB) ( 346 )  

    利用水提法和微生物发酵法制备丹参水提液和丹参发酵液,在生化水平、细胞水平、转录水平上探究二者抗氧化和美白能力。实验结果表明二者对1,1-二苯基-2-三硝基苯肼(DPPH)自由基均有良好的清除能力,丹参水提液清除率达到50%时的体积分数(IC50)为10.3%,丹参发酵液IC50值为2.9%,在相同体积分数下,丹参发酵液清除能力更佳。在细胞水平上,二者均表现出对过氧化氢诱导损伤细胞的保护作用,相对于损伤模型,细胞总抗氧化能力提高、丙二醛(MDA)含量和活性氧(ROS)含量降低、过氧化氢酶(CAT)活力提高。在转录水平上,相对于损伤模型,二者作用于细胞后CAT表达量均提高。在黑色素合成和酪氨酸酶活力抑制作用实验中,丹参水提液和丹参发酵液相对于空白对照均表现出良好的美白作用。总体而言,相对于丹参水提液,丹参发酵液在抗氧化功效和美白功效方面均表现更佳。

    Water extraction and microbial fermentation were used to prepare salvia miltiorrhiza water extract (SMWE) and salvia miltiorrhiza fermentation broth (SMFB). Their antioxidative and whitening abilities were studied at biochemical, cellular and transcriptional levels. The experimental results show that both have good scavenging ability to DPPH free radicals. The IC50 value of SMWE is 10.3%, and the IC50 value of SMFB is 2.9%. At the same volume fraction, the scavenging ability of SMFB is better. At the cellular level, both of them show protective effects against hydrogen peroxide-induced injury of cells. Compared with the injury model, the total antioxidant capacity of the cells is increased, the MDA content and ROS content are reduced, and the CAT activity is increased. At the transcription level, it is verified that CAT expression is both increased after the two acting on cells. In the experiments of melanin synthesis inhibition and tyrosinase activity inhibition, the SMWE and the SMFB both show good whitening effects compared with the blank control. In general, compared with SMWE, the SMFB is better in terms of antioxidative and whitening effects.

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    茴香酸在护肤品中溶解工艺的研究及其应用
    Study on the dissolution process of anisic acid and its application in cosmetic
    赵雪华
    2021 (10):  990-996.  doi: 10.3969/j.issn.1001-1803.2021.10.010
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    以控制变量法研究了茴香酸在护肤品中的溶解工艺及其应用。考察了L-精氨酸、1,2-己二醇、去离子水用量及溶解温度对茴香酸溶解工艺的影响。结果表明,茴香酸可完全溶解的质量配比范围为m(茴香酸):mL-精氨酸):m(1,2-己二醇):m(去离子水)=1:(0~1.5):(5~20):(0.5~100);其较佳质量配比范围为1:(0.8~1.5):(5~20):(0.5~2),此时所得溶液相对稳定。茴香酸较佳溶解温度为69~75 ℃。在L-精氨酸为0~0.2的质量配比条件下,分别配制了一款面霜和乳液类产品。两款产品均通过-15、25、40和48 ℃温度下的12周稳定性测试。显微镜测试表明,不同温度下,12周的面霜和乳液在水溶液中形成的乳液大小及其分布都较为均匀,长期稳定性较好。微生物挑战结果表明,面霜产品可通过1级防腐挑战,乳液产品可通过3级防腐挑战。

    The antibacterial effect of anisic acid gradually highlights its advantages in non-preservative skin care products. However, its insoluble property in water greatly limits its use in cosmetics. Therefore, in the production process of cosmetics, the problem of realizing and accelerating the dissolution of anisic acid needs to be further solved. In this paper, the dissolution process and application of anisic acid in cosmetic were studied by the control variable method. The effects of the dosage of L-arginine, 1,2-hexanediol, and deionized water, their dissolution time and temperature on the dissolution process of anisic acid were investigated. The better quality ratios among the influencing factors were screened out. The anisic acid was applied as a preservative to a face cream and a lotion, and their stability and microbial challenges were tracked. The results show that the mass ratio range of anisic acid that can be completely dissolved is anisic acid:L-arginine:1,2-hexanediol:deionized water=1:(0-1.5):(5-20):(0.5-100); and the optimal quality ratio range is 1:(0.8-1.5):(5-20):(0.5-2), with the obtained solution relatively stable. The optimal dissolution temperature of anisic acid is 69-75 ℃. Under the condition of the mass ratio of L-arginine of 0~0.2, a face cream and a lotion were prepared respectively. Both products have passed 12-week stability test at -15, 25, 40 and 48 ℃. Microscopic images show that the size and distribution of the emulsion formed in the aqueous solution of the face cream and lotion cream at different temperatures for 12 weeks are uniform and have good long-term stability. The results of the microbial challenge test show that the cream can pass the level 1 preservative challenge, and the lotion can pass the level 3.

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    专论与综述
    皮肤信息化的应用研究现状与展望
    Current situation and prospect of skin informatization
    张慧妍,崔雪莹,王小艺,孟宏,许继平
    2021 (10):  997-1002.  doi: 10.3969/j.issn.1001-1803.2021.10.011
    摘要 ( 209 )   HTML ( 7 )   PDF(1077KB) ( 419 )  

    皮肤作为一道屏障,美观与保护意义重大。从信息化角度出发,对皮肤指标与状态相关性,皮肤状态评价、皮肤指标预测、皮肤养护用化妆品决策等几个方面进行了应用研究现状综述。总结了目前采用的相关性、评价、预测及决策方法的特点和适用性,并对皮肤指标与人体健康、所关注皮肤领域问题间的相关性,皮肤检测分析系统研发等方向进行了展望。指出随着信息化技术的发展,图像、数据、专家经验等相对以往更容易获取、存储,使得采用信息化技术客观、系统地进行皮肤指标、状态的综合评价、预测、决策等研究成为可能。皮肤研究具有一定的复杂性,后续可融合机器学习等方法横向挖掘指标与问题间的非线性相关性,纵向提炼指标随时间的演化规律,在此基础上进行专家与消费者、检测数据协同的智能决策以科学选取化妆品实现对皮肤性能的改善。最后,指出利用方便采集的图像并结合云端服务器,研发高效、快速、具有自主知识产权的皮肤检测分析系统将是皮肤化妆品领域研究的一个重要方向。

    Skin as a barrier, is of great significance for the beauty and protection of human. A review of the research and application on the information in skin research was presented. It presents the correlation between skin index and body state, evaluation, prediction and decision making methods of cosmetics for the skin care to assist skin diagnosis and treatment system development and so on. The further research contents are also prospected, which include the characteristics of various skin evaluation methods, prediction and decision-making algorithms. And the correlation study of skin indexes with the human health and skin areas of concern is an important basis of the research and development of skin detection and analysis system, which highlight the role of informatization in helping the development of application fields. With the development of information, image, data and expert experiences are easier to obtain, analysis and store in computer than before, which makes it possible for the information technology to carry out the comprehensive evaluation, prediction and decision-making of skin index and state objectively and systematically. Skin research is complex, which could be influenced by many factors such as climate, region, sleeping and so on. In the future, skin informatization would integrate machine learning to mine the nonlinear correlation between research problems and indexes horizontally, extract the time evolution rules of index vertically, and make intelligent decision-making by experts and consumers cooperating. Data and image information will improve the study performance of the skin deeply and widely.

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    特殊化妆品安全技术评价常见问题分析
    Analysis of common problems in safety technical evaluation of special cosmetics
    钮正睿,李琳,苏哲,张凤兰,王钢力
    2021 (10):  1003-1010.  doi: 10.3969/j.issn.1001-1803.2021.10.012
    摘要 ( 311 )   HTML ( 18 )   PDF(961KB) ( 444 )  

    化妆品安全技术评价是化妆品监管体系中的重要环节。我国现行法规中将化妆品分为特殊化妆品和普通化妆品,按风险程度分类管理原则,对特殊化妆品实行注册管理,对普通化妆品实行备案管理。结合开展化妆品安全技术评价的工作实际,对影响特殊化妆品安全性的问题进行归纳和梳理,并结合具体案例开展分析,为化妆品产品研发、监管部门和技术机构开展相关工作提供借鉴。

    The use of cosmetics has a long history. Nowadays, cosmetics have become one of the most common consumer products in people’s lives. However, from the perspective of per capita consumption level of cosmetics, China’s per capita consumption still lags behind developed countries. With the development of economy, improvement of people’s consumption level and the change of consumption consciousness, cosmetics industry has a broader development space. The production of cosmetics is a sunrise industry in economic development. Different from drugs, cosmetics mainly play the role of beautifying and embellishing life. Safety is the basic feature for cosmetics, and the efficacy of the products follows. Enterprises should put product safety in the first place in the progress of researching and developing cosmetics. China’s current regulations divide cosmetics into special cosmetics and ordinary cosmetics. Special cosmetics include hair dyeing cosmetics, perm cosmetics, skin bleaching and skin whitening cosmetics, sunscreen cosmetics and anti-hair loss cosmetics, as well as the cosmetics that claim new effects. Compared with ordinary cosmetics (such as cosmetics that claim to have cleansing or moisturizing effects), special cosmetics have a higher risk to the consumers. Cosmetics are managed according to the risk degree in China. Special cosmetics are subject to registration management, and for ordinary cosmetics, record management are carried out. In China, the cosmetics safety evaluation department plays an important technical support role in the product safety review process. The safety technical evaluation for cosmetics is a key step in China’s cosmetics supervision system. Among the system, the evaluation for special cosmetics safety is the main part. Under the new framework of “Regulations on Supervision and Administration of Cosmetics”, higher requirements are put forward for cosmetic registrants and record holders, especially in quality management system, adverse reaction monitoring and evaluation, etc. Cosmetic applicants and technical evaluators should strengthen their studies, and pay more attention to the issues that affect safety in application details. Based on the practical experience of cosmetic safety technical evaluation, the author summarized, sorted out and analyzed issues affecting safety of special cosmetics according to specific cases, which can provide reference for cosmetic product research and development, regulatory agencies and technical institutions to carry out related work.

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    化妆品中铅、汞元素检测方法的研究进展
    Research progress on detection methods of lead and mercury in cosmetics
    蒲苏丹,刘燕茹,孟佩俊,李淑荣,罗利霞
    2021 (10):  1011-1017.  doi: 10.3969/j.issn.1001-1803.2021.10.013
    摘要 ( 304 )   HTML ( 20 )   PDF(936KB) ( 580 )  

    随着人们健康生活意识的不断提升,化妆品中铅、汞等重金属元素超标引发的健康问题受到了高度关注,其检测方法也不断推陈出新。文章综述了化妆品中铅、汞元素检测的原子吸收光谱、原子荧光光谱、电感耦合等离子体发射光谱、电感耦合等离子体质谱、电化学分析等常规方法以及汞分析、X射线荧光光谱、激光诱导击穿光谱等快速检测方法的研究现状及进展,同时比较了不同方法间灵敏度和准确度的差异,为化妆品中铅、汞检测方法创新提供思路。

    With the gradual improvement of people’s living standards, cosmetics have come into the life. The lead and mercury contained in cosmetics have a whiting effect on skin. However, an excess can cause great harm to people’s health. So, there are relevant laws and regulations at home and abroad that strictly limit the content of lead and mercury in cosmetics. Moreover, the health issues caused by excessive heavy metal elements such as lead and mercury in cosmetics have drawn a widespread public attention, and the detection methods have been constantly updated. Present situation and progress of research on detecting lead and mercury in cosmetics are summarized, including not only conventional methods, such as atomic absorption spectroscopy, atomic fluorescence spectroscopy, inductively coupled plasma emission spectroscopy, inductively coupled plasma mass spectrometry, and electrochemical analysis, but also rapid detection methods, as of mercury analyzer, X-ray fluorescence spectroscopy, and laser induction spectroscopy. However, it is important to figure out which detection technology is the best way to test the excessive lead and mercury content in cosmetics. Actually, whether factory detection or sales process detection, it is necessary to choose an efficient, fast and low-cost detection methods for lead and mercury element in cosmetics. Based on the paper, in contrast to the differences of sensitivity and accuracy between various methods, it is found that electrochemical analysis technology exhibits outstanding advantages, such as simple, fast, and low-cost. What’s more, with the continuous innovation of its detection materials, it is of enormous potential for electrochemical method in the detection of heavy metals. This method provides a new idea for detecting lead and mercury in cosmetic.

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    分析与检测
    高效液相色谱法同时测定防晒类化妆品中23种禁限用组分的含量
    Simultaneous determination of 23 prohibited or restricted components in sunscreen cosmetics by high performance liquid chromatography
    尚姝,冯有龙,方方
    2021 (10):  1018-1025.  doi: 10.3969/j.issn.1001-1803.2021.10.014
    摘要 ( 218 )   HTML ( 9 )   PDF(1086KB) ( 405 )  

    建立了高效液相色谱法同时测定防晒类化妆品中23种禁限用组分的含量。样品加混合溶剂或四氢呋喃溶解后,混匀,超声提取30 min,用混合溶剂或四氢呋喃稀释至刻度,用微孔滤膜过滤,经Kromasil C18柱分离,以0.1%甲酸-甲醇-四氢呋喃为流动相进行梯度洗脱,流速为1.0 mL/min,柱温为35 ℃,检测波长为311 nm,用标准曲线法进行定量计算。方法学研究表明,23种防晒剂禁限用组分在一定浓度范围内与峰面积的线性关系良好,R值均大于0.998 4,方法检出限为0.01%~0.04%。在低、高两种加标水平下,两种基质(防晒霜和唇膏)中23种防晒剂禁限用组分的回收率均在85.6%~113.2%之间,RSD在0.4%~5.4%之间,说明本方法对测定禁限用组分的准确性较高。本方法在《化妆品安全技术规范》(2015年版)收载方法基础上进行了优化,使检测过程中各组分的稳定性更好。

    High performance liquid chromatography (HPLC) method for simultaneous determination of 23 prohibited or restricted components in sunscreen cosmetics was established. The sample was dissolved and mixed with tetrahydrofuran or a mixed solvent, extracted by sonicating for 30 min, diluted with tetrahydrofuran or a mixed solvent, and filtered by a microporous membrane. For HPLC analysis, the sample was separated by Kromasil C18 column, and gradient elution was performed with 0.1% formic-methanol-tetrahydrofuran as the mobile phase, with the flow rate of 1.0 mL/min, column temperature of 35 ℃, detection wavelength of 311 nm. The quantitative determination was applied by standard curve method. The results show that there is a good linear relationship between the concentration of 23 prohibited or restricted components and the peak area is in a certain range, with the R values all greater than 0.998 4. The detection limits of the method are 0.01%-0.04%. At low and high spiked levels, the recoveries of the two substrates (sunscreen and lip balm) ranged from 85.6%-113.2%, with RSDs ranging from 0.4%-5.4%. This method is optimized on the basis of the loading method in Safety and Technical Standards for Cosmetics (2015 Edition), so that the stability of each component in the detection process is better. On the basis of the “specification” detection method in this paper, the extraction solvent and the kind of mobile phase of the test sample solution is optimized. The new method can simultaneously determine amino acid and diphenyl ketone-2 of 23 kinds of sunscreen, improve the efficiency of the detection, enhance the stability of the component under test condition and ensure the stability of the measured component accuracy. In this paper, HPLC method was used to establish a simultaneous detection method for 23 kinds of prohibited or restricted sunscreen substances, and the extraction solvents and mobile phase types of the tested solutions were optimized. The new method overcomes the inaccuracy of the detection results caused by the easy oxidation of cresol trazole trisiloxane and other contained detection methods in the Code. The new method can simultaneously determine 23 kinds of sunscreens such as p-aminobenzoic acid and diphenylketone-2, which greatly improves the detection efficiency. The new method is proved to be accurate and repeatable, and is suitable for the inspection and detection of sunscreen cosmetics.

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    ICP-MS法测定人源化胶原蛋白中9种微量元素
    Simultaneous quantitative determination of the nine trace elements in human collagen by ICP-MS
    王慧,董庆斌,杨丽萍,代林涛
    2021 (10):  1026-1031.  doi: 10.3969/j.issn.1001-1803.2021.10.015
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    建立同时定量测定人源化胶原蛋白中Cr,Fe,Ni,Cu,As,Mo,Cd,Hg和Pb 9种微量元素的方法。对同时测定各元素的线性范围进行考察,并对方法学进行了验证。结果表明,9种微量元素在线性范围内线性良好,相关系数大于0.99,检出浓度为0.1~4.1 ng/kg,定量浓度为0.5~135 ng/kg,精密度RSD为1.8%~6.0%,回收率为88.5%~107.9%。本方法具有高效、简便、准确等优点,可为人源化胶原蛋白生产过程中的质量监测提供方法参考。

    A method for simultaneous quantitative determination of Cr, Fe, Ni, Cu, As, Mo, Cd, Hg and Pb in human collagen was established. Also, the linear range of each element was investigated. Moreover, this method of quantitative determination was verified. The results show that the nine trace elements present good linearity in the linear range, the correlation coefficient is more than 0.99, the limit of quantitation is 0.1-4.1 ng/kg, the quantitative concentration is 0.5-135 ng/kg, the precision RSD is 1.8%-6.0%, and the recovery is 88.5%-107.9%. This method has advantages of high efficiency, simplicity and accuracy, which can provide a reference for the quality monitoring in the production process of human collagen.

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    高效液相色谱法测定化妆品中视黄醇等9种组分
    Detection of nine components including retinol in cosmetics by high performance liquid chromatography
    刘玉玲,林亮亮,潘小红,赵薇,殷帅
    2021 (10):  1032-1038.  doi: 10.3969/j.issn.1001-1803.2021.10.016
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    建立高效液相色谱法测定化妆品中阿达帕林、维甲酸、异维甲酸、维胺酯、他扎罗汀、视黄醇、视黄醇醋酸酯、视黄醇丙酸酯、视黄醇棕榈酸酯9种成分的含量。以甲醇-异丙醇(体积比55∶45)为提取液,用高效液相色谱仪进行分析,以5 mmol/L乙酸铵(pH值=4.5)-甲醇-异丙醇为流动相,流速为1.0 mL/min,采用色谱柱CAPCELL PAKC18 (4.6 mm×250 mm×5 μm)分离,在238,325和355 nm检测波长下经HPLC检测,同时对提取剂和提取时间、流动相比例、检测波长等条件进行优化。视黄醇、视黄醇醋酸酯、视黄醇丙酸酯、视黄醇棕榈酸酯、他扎罗汀、异维甲酸、维甲酸、维胺酯和阿达帕林的检出限分别为2.01、0.95、1.72、1.65、0.78、1.23、1.94、5.29和0.22 μg/g,定量限分别为6.70、3.17、5.73、5.50、2.60、4.10、6.47、17.63和0.73 μg/g,高、中、低不同质量浓度的加标提取回收率在80.56%~112.63%之间,相对标准偏差在0.18%~5.85%之间,在0.12~29.19 mg/L的质量浓度范围内线性关系良好(R2>0.995 9)。该方法快速准确,可适用于化妆品中视黄醇类成分含量的测定。

    A method for the simultaneous determination of 9 components (adapalin, tretinoin, isotretinoin, viaminate, tazarotene, retinol, retinyl acetate, retinyl propionate, retinol palmitate) in cosmetics by high performance liquid chromatography was established. The effects of extraction solvents on the retinol components were explored, and it is found that when the extraction solvent is methanol-isopropanolas (volume ratio 55∶45), the recovery rate of various retinol components can reach the best level. Meanwhile, to obtain higher sensitivity, the acidic mobile phase methanol-isopropanolassystem was used to separate the retinol components. It is found that when the pH is 4.5 and the concentration is 5 mmol/L, the resolution of the 9 retinol components can achieve the best results. Finally, the 9 retinol components were separated by CAPCELL PAK C18 (4.6 mm×250 mm×5 μm) column using 5 mmol/L ammonium acetate (pH=4.5)-methanol-isopropanolas as the mobile phase, and qualitative and quantitative analysis was performed by high performance liquid chromatography with DAD detection under the detection wavelength of 238, 325 and 355 nm. The flow rate was 1.0 mL/min. The results show that there is a good linear relationship in the range of 0.12-29.19 mg/L between concentration and peak area with R2 greater than 0.995 9. The limits of detection for adapalin, tretinoin, isotretinoin, viaminate, iazarotene, retinol, retinyl acetate, retinyl propionate, and retinol palmitate are 2.01, 0.95, 1.72, 1.65, 0.78, 1.23, 1.94, 5.29 and 0.22 μg/g, respectively, and the limits of quantification are 6.70, 3.17, 5.73, 5.50, 2.60, 4.10, 6.47, 17.63 and 0.73 μg/g, respectively. The average recoveries are from 80.56% to 112.63%, with relative standard deviations in the range of 0.18% to 5.85%. This method has advantages such as simple pretreatment, high sensitivity, rapid and accurate. It is suitable for the simultaneous determination.

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