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    2022年, 第52卷, 第10期 刊出日期:2022-10-22 上一期    下一期
    基础研究
    发酵莲花花瓣美白功效提升及作用机制研究
    Enhancement of anti-melanogenic properties of lotus (Nelumbo nucifera) petals extract treated by Lactobacillus plantarum and its mechanism
    赵胜男,郭苗苗,蔡孟浩,洪民华,吕智,安法梁
    2022 (10):  1029-1039.  doi: 10.3969/j.issn.1001-1803.2022.10.001
    摘要 ( 375 )   HTML ( 34 )   PDF(2104KB) ( 313 )  

    随着现代生物工程技术快速发展,利用发酵技术提高草药提取物在食品和化妆品添加剂领域的生物活性已成为新趋势。在本研究中,以蘑菇酪氨酸酶活性和黑色素形成为评价指标,对5种益生菌的莲花提取物(LPE)发酵产物进行活性筛选。结果显示植物乳杆菌CGMCC 1.124发酵产物(FLPE)具有酪氨酸酶抑制活力;在A-MSH诱导的小鼠黑色素瘤细胞(B16F10)美白模型中,经50 μg/mL FLPE处理的B16F10黑色素含量为模型对照组的86%±4.6%。为进一步阐明FLPE主要活性成分,利用HPLC,NMR和LC-MS对莲花提取物发酵前后产物中的主要黄酮类化合物进行定性定量分析。结构分析和生物活性评价结果表明,山奈酚-3-O-β-D-葡萄糖苷(49.8%,94.22 mg/g)和槲皮素-3-O-β-D-葡萄糖醛酸(13.6%)生物转化为两个生物活性苷元-槲皮素(14.4%,26.43 mg/g)和山奈酚(60.9%,70.76 mg/g)。在这些单体中,槲皮素通过调节酪氨酸酶活性、黑素发生相关酶(TYR,TRP-1和TRP-2)和小眼畸形相关转录调控因子(MITF)的表达抑制黑素形成。总体而言,利用植物乳杆菌CGMCC 1.124发酵提高了莲花提取物美白功效,转化生成的槲皮素是植物乳杆菌发酵产物抑制黑色素合成的物质基础之一。

    Considering the growing evidence that microbial fermentation, as an optimum processing method, can improve the biological activity of herbal extracts in food and cosmetic additives fields. In recent years, owing to the unique aroma and pharmacological activity, lotus petals extract has been utilized in the preparation of cosmetic and food. However, none is available on the improvement of anti-melanogenic activity in the microorganism-fermented lotus petals extract (LPE). Thus, in this study, it is hoped to enhance anti-melanogenic properties of lotus petals extract by using fermentation technology and clarify its mechanism of action. We screened five probiotics (L.plantarum CGMCC 1.124, L.fermentum DSMZ 20052, Bacillus subtilis CGMCC 1.943, B.natto CGMCC NO. 19463 and B.natto CGMCC NO. 19462) to ferment LPE with evaluating for their anti-melanogenic activity by mushroom tyrosinase and melanin formation inhibition assays, hoping to establish a new method to improve the anti-melanogenic activity of LPE. The results indicate that LPE fermented with L.plantarum CGMCC 1.124 (FLPE), shows enhancement on anti-mushroom tyrosinase and anti-melanogenic activity in A-MSH-stimulated B16F10 melanocytes. In particular, compared with A-MSH incubation alone, co-incubation with 50 μg/mL FLPE reduces the melanin production to 86%±4.6%. To determine the main effectors of the anti-melanogenesis of FLPE, primary flavonoids from LPE and FLPE were isolated and determined by high performance liquid chromatography (HPLC), nuclear magnetic resonance (1H NMR, 13C NMR) and liquid chromatography mass spectrometry (LC-MS) analyses. The results of structure analysis and bioactivity evaluation show that flavonoid glycosides kaempferol-3-O-β-D-glucopyranoside (49.8%, 94.22 mg/g) and quercetin-3-O-β-D-glucuronide (13.6%) are bio-transformed to two bioactive aglycones, quercetin (14.4%, 26.43 mg/g) and kaempferol (60.9%, 70.76 mg/g). Among these monomers, quercetin and kaempferol decrease the mushroom tyrosinase activity, but only quercetin shows anti-melanogenic activity by suppressing tyrosinase activity in B16F10 cells, regulating the mRNA expressions of melanogenesis-related enzymes (TYR, TRP-1 and TRP-2) and microphthalmia-associated transcription factor (MITF) and reducing the protein contents of TYR, TRP-1 and MITF in a dose-dependent manner. These data suggest that FLPE has a potential for skin whitening with quercetin as a functional compound. These results maybe contribute to developing healthy food and cosmetic, and expand the range of application of lotus petals.

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    姬塬油田耐温抗盐表面活性剂增注体系研究
    Research and application of a temperature-resistant and salt-resistant surfactant injection system for Jiyuan Oilfield
    陆小兵,郑延成,刘小宁,王伟,兰乐芳
    2022 (10):  1040-1048.  doi: 10.3969/j.issn.1001-1803.2022.10.002
    摘要 ( 199 )   HTML ( 19 )   PDF(1440KB) ( 347 )  

    为解决姬塬油田超低渗油藏中温、高矿化度储层注水开发效果差的问题,合成了一种新型阴-非离子表面活性剂醇醚磺酸盐DES,并与油酸酰胺型甜菜碱两性表面活性剂HGC复配,研制出一种耐温抗盐型高效复合表面活性剂增注体系。对体系性能进行了室内评价,结果表明:体系具有良好的耐温抗盐性能,在温度100~110 ℃、矿化度65.5 g/L时,油水界面张力为10-3 mN/m数量级;在75 ℃,矿化度高于120 g/L时,油水界面张力为10-3 mN/m数量级;在110 ℃下老化30 d后仍能保持超低界面张力水平;体系的动态吸附量较小,预示其在地层中的吸附损失较少;当注入0.2 PV的增注体系时,能够使岩心水驱后的降压率达到18.39%;当注入0.6 PV的增注体系时,能够使岩心水驱后的降压率达到30.54%。现场应用结果表明,措施后注水井注入压力下降3.0 MPa,单井累计增注11 780 m3,降压增注效果显著。

    The enhancement of oil recovery efficiency by water flooding has been restricted by the harsh conditions of the reservoirs (medium temperature, high salinity and low permeability) in Jiyuan Oilfield. Herein, a new type of anionic-nonionic surfactant, fatty alcohol ether sulfonate (DES), was synthesized and compounded with an oleate amide betaine surfactant (HGC) that was derived from oleic acid. Thus, a flooding agent containing DES/HGC that could withstand high temperature and salinity was developed and systematically evaluated. The results confirmed the well temperature- and salt-resistance of the flooding agent. At a temperature range of 100-110 ℃ and salinity of 65.5 g/L, an ultra-low interfacial tension (~10-3 mN/m) between the oil and the surfactant solution was obtained. At 75 ℃, an interfacial tension of ~10-3 mN/m could also be reached when the salinity was above 120 g/L. The ultra-low interfacial tension level could still be maintained after being aged at 110 ℃ for 30 days; the dynamic adsorption of the system was weak, indicating that the adsorption loss of the surfactants in the formation was small; when 0.2 PV and 0.6 PV of flooding agent were injected into the core samples, the pressure of water flooding could be decreased by 18.39% and 30.54%, respectively. The field tests showed that the injection pressure of the water injection could be decreased by 3.0 MPa, and the cumulative injection of a single well was increased by 11 780 m3, indicative of remarkable effects of pressure reduction and injection increase.

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    科技讲座
    常用化妆品成型技术(Ⅳ)——粒微效强:粉剂
    Common cosmetic preparation technologies (Ⅳ) Powerful particulates: Powders
    包杰,冯云,樊建茹,石晶,徐桂云,范金石
    2022 (10):  1049-1054.  doi: 10.3969/j.issn.1001-1803.2022.10.003
    摘要 ( 408 )   HTML ( 22 )   PDF(1070KB) ( 484 )  

    粉剂是指外观呈粉状或粉质块状的干剂,通常是将功效成分、辅料及适当助剂一起混合粉碎得到的,广泛应用于化妆品、口腔卫生用品及医药、农药化肥、军工、油墨、印刷、化工、材料、建筑、饲料等多个行业领域。粉剂的性能主要由功效成分的性质决定,但也与粉剂的颗粒大小与形状、比表面积、密度、吸湿性、流动性等特性密切相关。本文介绍了粉剂的特性、生产设备、生产工艺,并着重介绍了粉剂在美容、美白、防晒化妆品及面膜、药妆和口腔卫生用品方面的应用情况,并简析了粉剂当前存在的问题、未来研发重点和发展趋势。

    Powder refers to the dry preparation made up of particulate matters or pressed fine granules, usually prepared by mixing, pulverizing the functional ingredients together with auxiliary excipients and appropriate additives. For a long time, powders have been widely used in medicine, pesticides, cosmetics, oral hygiene, fertilizers, printing ink, chemicals, materials, coating, fodder and other fields. Beyond question, the functions of powders are mainly determined by the properties of the key active ingredients, but the characteristics of the powder, such as particle size, particle shape, specific surface area, density, hygroscopicity and flowability, are also directly related to the actual effects of the powder. Herein, the characteristics, the production equipments and the production process of powders were introduced. Furthermore, some typical applications of powders in beauty cosmetics, whitening cosmetics, sunscreen cosmetics, facial masks, cosmeceuticals and oral hygiene products in recent years were introduced. Finally, several environmental, safety items during the production and use of powders were mentioned. The priorities in research and development, and the directions of development for powders in the future were also pointed out.

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    开发与应用
    C16格尔伯特醇聚氧烷烯醚硫酸盐的制备及其界面性能研究
    Study on the preparation of C16 Guerbet alcohol polyoxyalkylene ether sulfate and its interfacial properties
    陈琪,冉立君,陈钊,崔正刚
    2022 (10):  1055-1061.  doi: 10.3969/j.issn.1001-1803.2022.10.004
    摘要 ( 192 )   HTML ( 8 )   PDF(1217KB) ( 366 )  

    用C16格尔伯特醇经共聚加成环氧丙烷(PO)和环氧乙烷(EO),再经氨基磺酸硫酸化合成了一种支链烷基醇醚硫酸盐(C16GA-PES)。这种新型阴-非复合型表面活性剂具有优良的水溶性、耐盐性和表面活性。45 ℃下溶于大庆地层水,单独即可将大庆轻质原油/地层水界面张力降至超低;对稍重质的大庆三类油层油,使用该表面活性剂与少量亲油性更强的表面活性剂混合,亦可将界面张力降至超低。这种新型结构表面活性剂吸附在油/水界面形成的单分子层具有从强亲油到弱亲油-弱亲水再到强亲水的过渡结构,而双烷基链又赋予单分子层较高的烷基链密度,从而增强了单分子层与油分子的相互作用,易于将原油/水界面张力降至超低。与相应的嵌段中间体相比,共聚所得非离子中间体黏度显著降低,便于管道输送并且有利于采用SO3气体降膜式硫酸化工艺制备硫酸盐。

    A new anionic-nonionic surfactant with branched hydrophobic group was prepared using C16 Guerbet alcohol by co-polymerization of propylene oxide (PO) and ethylene oxide (EO) followed by sulfation with aminosulfonic acid. This surfactant (C16GA-PES) shows excellent aqueous solubility, good tolerance to inorganic electrolytes such as sodium chloride (NaCl) and calcium chloride (CaCl2), and good surface activity (cmc=1.15×10-6 mol/L). When dissolved in Daqing formation water (pH=8-9) with a total salinity of 6 788 mg/L, including 23 mg/L Ca2+ and 31 mg/L Mg2+ at 45 ℃, the C16GA-PES solely can reduce the interfacial tension (IFT) between Daqing light crude oil and formation water to ultralow (<0.01 mN/m); for the slightly heavy crude oil from the third type of reservoir in Daqing oilfield, ultralow IFT can be achieved by mixing the C16GA-PES with a small fraction of more hydrophobic surfactant, 1,3-didecyl glyceryl ether hydroxypropyl sulfobetaine (diC10GE-HSB). The new surfactant adsorbs at the oil/water interface constituting a monolayer which has high alkyl chain density and a transition structure from strongly hydrophobic to weak hydrophobic-weak hydrophilic and to strong hydrophilic, resulting in strong interactions between the monolayer and oil molecules and making ultralow IFT easily achievable. It is also noticed that, the nonionic intermediate produced by co-polymerization of PO and EO has low viscosity, which is beneficial to pipeline transport and sulfation with SO3/air mixture.

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    海上油井高效经济钡锶垢除垢剂体系评价及除垢工艺研究
    Evaluation of efficient and economical Ba/Sr scale remover and descaling technology for offshore oil wells
    吴绍伟,程利民,万小进,梁玉珠,张亮,康万利
    2022 (10):  1062-1071.  doi: 10.3969/j.issn.1001-1803.2022.10.005
    摘要 ( 177 )   HTML ( 10 )   PDF(1286KB) ( 244 )  

    海上油井钡锶垢清除难度大、作业费用高,需要通过优化除垢剂配方和改进除垢工艺来降低除垢成本。针对涠洲油田群典型井下工况,采用真实垢样开展了除垢剂溶垢实验,从保持除垢效果降低药剂用量和保持药剂用量提高除垢效果两个角度,研发和改进了除垢剂配方;提出了除垢作业与修井作业二合一的工艺改进新思路,初步论证了除垢剂与修井液合二为一的可能性。结果表明,现用药剂SD-132和优选的新剂DTPA的用量降低至8%仍可满足除垢指标要求;研发的以DTPA为主剂的新剂改进配方,在相同质量分数(16%)下比现剂溶垢量可提高13.08%,现剂添加2%~4% DTPA后,溶垢量也可提高14.49%,且新配方对不同类型垢样均适用;除垢剂与修井液二合一具有一定可行性,两者复配后仍可保持良好的除垢和储保性能,若能实现修井作业同时除垢,除垢剂和施工成本将会大大降低,将大幅提高海上油井钡锶垢除垢工艺的经济性。

    Due to the difficulty in removing BaSO4/SrSO4 scale from offshore oil wells and the high operating costs, it is necessary to optimize the formula of descaling agent and the descaling process to reduce the scale removal cost. A series of descaling experiments were conducted referring to the typical bottom-hole conditions of the oil wells in Weizhou Oilfield. New formulas of descaling agent were developed, and the descaling agent currently used in field was improved, from the point of view of maintaining the descaling effect to reduce the amount of descaling agent or maintaining the amount of descaling agent to improve the descaling effect. A novel concept to improve the descaling process was proposed, in which the descaling operation was combined with the workover operation, and the feasibility thereof was preliminarily assessed. The results show that, the dosage of the current agent SD-132 and the preferred new agent DTPA can be reduced to 8% and still meet the descaling index requirements. The amount of scale dissolved by the developed new formula containing DTPA can be increased by 13.08% compared with the current agent SD-132 at the same mass fraction (16%). After adding 2%-4% DTPA to the current agent SD-132, the amount of scale dissolved can also be increased by 14.49%. The new formula is applicable to different types of scale samples. The combination of descaling agent and workover fluid has a certain feasibility. The combined fluid can still maintain good descaling and formation protection performance. If the workover can achieve descaling at the same time, the cost for descaling agent and operation will be greatly reduced. The economy of the Ba/Sr scale descaling process for offshore oil wells will be greatly improved.

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    虫草素纳米乳液制备及对皮肤光老化修复机制研究
    Preparation of cordycepin nanoemulsion and its repair mechanism on the photoaged skin
    张虎成,杨国伟,杨军,范海涛,罗帅,刘霖颖
    2022 (10):  1072-1080.  doi: 10.3969/j.issn.1001-1803.2022.10.006
    摘要 ( 229 )   HTML ( 19 )   PDF(2038KB) ( 320 )  

    将虫草素(cordycepin)作为功效成分制作成纳米乳液,并研究了虫草素纳米乳液配方工艺、质量初步评价和对皮肤光老化修复机制。通过绘制伪三元相图,确定虫草素纳米乳液配方,考察纳米乳粒径、黏度、稳定性,以及虫草素稳定性。利用紫外线照射新西兰兔子皮肤,检测皮肤中的超氧化物歧化酶(SOD)、谷胱甘肽(GSH)、过氧化氢酶(CAT)活力和丙二醛(MDA)的含量。结果表明,乳化剂和助乳化剂质量比(Km)为2∶1时得到的纳米乳液较稳定,虫草素纳米乳平均直径为374 nm,黏度为(9.33±0.14) mPa·s,具有良好的离心稳定性、稀释稳定性、长期稳定性和温度稳定性;虫草素1~8个月维持在(12.006±0.025) mg/g,RSD在1%以内,第9个月开始减少;使用虫草素纳米乳液实验组4的SOD、CAT活性和GSH含量稍低于对照组,显著高于实验组1、2和3 (P<0.01),对照组和实验组4的MDA含量均明显低于实验组1、2和3 (P<0.01)。虫草素纳米乳液具有较好的稳定性、黏度和粒径大小,可以有效缓解紫外线照射引起的皮肤衰老。

    Cordycepin was used as an effective component to prepare nanoemulsion. The formulation process, preliminary quality evaluation and skin photoaging repair mechanism of cordycepin nanoemulsion were studied. By drawing the pseudo ternary phase diagram, the formula of the nanoemulsion was determined. The particle size, viscosity, and stability of the nanoemulsion were investigated. The activity of superoxide dismutase (SOD), glutathione (GSH), catalase (CAT) and the content of malondialdehyde (MDA) in the skin of New Zealand rabbits were measured. The results show that the nanoemulsion is stable when the Km of surfactant and co-surfactant is 2∶1. The average diameter of cordycepin nanoemulsion is 374 nm and the viscosity is (9.33±0.14) mPa·s. It has good centrifugal stability, dilution stability, long-term stability and temperature stability. Cordycepin can be maintained at (12.006±0.025) mg/g for 1-8 months with the RSD within 1%, and it begins to decrease in the ninth month. The activities of SOD, CAT and GSH in group 4 using cordycepin nanoemulsion are slightly lower than those in the control group, significantly higher than those in groups 1, 2 and 3 (P<0.01). The MDA in the control group and group 4 are significantly lower than those in groups 1, 2 and 3 (P<0.01). Cordycepin nanoemulsion has good stability, viscosity and particle size, and can effectively alleviate skin aging caused by ultraviolet radiation. This study aims to lay a theoretical foundation and provide direction for the further development of the function of cordycepin nanoemulsion.

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    纳米甲壳素的快速制备及其乳化性能研究
    Rapid preparation of nano-chitin for stabilizing Pickering emulsions
    宦静静,王碧佳,毛志平,隋晓锋
    2022 (10):  1081-1087.  doi: 10.3969/j.issn.1001-1803.2022.10.007
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    简化磷酸溶解再生制备纳米甲壳素的工艺,避免大量溶剂的使用、缩短制备时间以及提高产率。采用X射线衍射、透射电镜和电感耦合等离子体发射光谱仪对甲壳素及再生纳米甲壳素进行了表征。以辛酸/癸酸甘油三酯(GTCC)作为油相,用纳米甲壳素作为Pickering乳液稳定剂,制得水包油(O/W)型Pickering乳液。通过各类表征证明该方法制备的所有纳米甲壳素均可以乳化GTCC得到稳定的Pickering乳液(纳米甲壳素含量为0.2%)。随后其乳液的流变行为表明纳米甲壳素能很好地吸附在油水界面上,并且稳定Pickering乳液。

    Nano-chitin was prepared by treating raw chitin with phosphoric acid (H3PO4) for 40 min followed by high-pressure homogenization. This method could save chemical reagents, shorten the preparation process and increase the yield as compared with the previous preparation method. The chitin and regenerated nano-chitin (RCh) were characterized by XRD, TEM and inductively coupled plasma atomic emission spectrometry. The experimental conditions of preparation were optimized, such as the minimum concentration of phosphoric acid to dissolve chitin and the maximum concentration of chitin that could be dissolved by different concentrations of phosphoric acid. The RCh suspension thus prepared was used to stabilize caprylic/capric triglyceride (GTCC) to fabricate oil-in-water Pickering emulsions. The emulsions were characterized on an optical microscope, a dynamic laser scattering size analyzer and a rheometer. All the RCh prepared with this method could well stabilize Pickering emulsions (RCh content was only 0.2%). The RCh adsorbed on the O/W interface could stabilize the Pickering emulsions. The rheological behaviors of Pickering emulsions indicated that, the entanglement of RCh enhanced the structure of the emulsions as well as their resistance to deformation. The energy storage modulus and loss modulus remained constant with the change of scanning frequency at a fixed stress, and no intersection point was found in the frequency range, which indicated that the emulsions were stable and had “gel-like” behavior. All emulsions showed shear thinning behavior. RCh was effective in preventing droplet coalescence and could form stable Pickering emulsions when GTCC mass fraction was not higher than 60%.

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    PoPD-TiO2-GO复合光催化剂在化工染料废水吸附降解中的应用
    Application of PoPD-TiO2-GO composite photocatalyst in adsorption and degradation of chemical dye wastewater
    张勤,石秋红
    2022 (10):  1088-1093.  doi: 10.3969/j.issn.1001-1803.2022.10.008
    摘要 ( 158 )   HTML ( 5 )   PDF(1219KB) ( 280 )  

    采用石墨粉、磷酸、浓硫酸等试剂制备TiO2-GO复合光催化剂,并在该催化剂基础上添加邻苯二胺制得PoPD-TiO2-GO复合光催化剂,同时制备活性黑KN-B化工染料废水,向染料废水中依次加入两种催化剂,并通过光反应仪器、热重分析仪等仪器分析催化剂吸附降解能力。经实验验证:两种催化剂中石墨烯添加量过大虽然会增加比表面积,但会导致吸光度下降,添加3%石墨烯的两种催化剂效果较佳;随着吸附时间的增长,PoPD-TiO2-GO的吸附率与脱色率明显高于TiO2-GO,且两种催化剂的用量越大,对化工染料废水的脱色能力就越强;PoPD-TiO2-GO经4次循环降解后脱色率依然保持在70%以上,当选取多种废水染料实验时,PoPD-TiO2-GO均能够维持较高的脱色率,因此,PoPD-TiO2-GO复合光催化剂的降解性能较好,可以降解多种染料废水,同时PoPD-TiO2-GO的综合吸附降解能力要高于TiO2-GO。

    TiO2-GO composite photocatalyst was prepared using graphite powder, phosphoric acid and sulfuric acid. On the basis of this catalyst, o-phenylendiamine was added to prepare the PoPD-TiO2-GO composite photocatalyst. The simulated chemical dye wastewater containing reactive black KN-B was prepared. These two new catalysts were added to the chemical dye wastewater, and the abilities of the catalysts in adsorption and degradation were analyzed on the light reaction apparatus and thermogravimetric analyzer. The experimental results show that, excessive addition of graphene in the two catalysts will increase the specific surface area but will lead to the decrease of absorbance. Therefore, the two catalysts with 3% graphene have better effects; With the increase of adsorption time, the adsorption rate and decolorization rate of PoPD-TiO2-GO are significantly higher than those of TiO2-GO. The greater the amount of the two catalysts, the stronger the decolorization capacity to chemical dye wastewater; the decolorization rate of PoPD-TiO2-GO remains above 70% after four cycles of degradation. When a variety of wastewater dyes are selected for the experiment, PoPD-TiO2-GO can still maintain a high decolorization rate. Therefore, the degradation performance of PoPD-TiO2-GO photocatalyst is good, which can degrade a variety of dye wastewater. In addition, the comprehensive ability of adsorption and degradation of PoPD-TiO2-GO is higher than that of TiO2-GO.

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    表面活性剂及液体洗涤剂终极生物降解的方法与性能研究
    Study on the methods and performance of ultimate biodegradation of surfactants and liquid detergents
    洪玉倩,葛赞,洪郑,雷小英,黄晴
    2022 (10):  1094-1099.  doi: 10.3969/j.issn.1001-1803.2022.10.009
    摘要 ( 298 )   HTML ( 11 )   PDF(1141KB) ( 227 )  

    生物降解性能分为初级生物降解性能和终极生物降解性能两种,是考察表面活性剂对环境影响的重要因素。随着社会的发展,人们对环境的重视程度日益加深,而目前系统地对常用表面活性剂的终极生物降解性能研究较少。在此,采用总有机碳(TOC)分析仪结合GB/T 21856—2008《化学品快速生物降解性二氧化碳产生试验》对10种常用表面活性剂和市场上不同品牌和类别的液体洗涤剂进行终极生物降解性能研究,考察它们对环境的影响。该方法简单易操作,重复性高。分析结果表明,几种常见的表面活性剂,降解率都在60%以上,符合环境要求。其中除LAS外,其余几种皆大于80%,终极降解性能优异。市场上一些洗涤剂产品降解率也都大于80%,终极生物降解性能优。

    Biodegradability is classified into primary biodegradability and ultimate biodegradability, which is an important factor to assess the impact of surfactants on the environment. With the development of society, people have paid more and more attention to the environment, and however, there are few systematic studies on the ultimate biodegradation performance of commonly used surfactants. Herein, a total organic carbon (TOC) analyzer combined with GB/T 21856—2008 “Chemical—Ready biodegradability—CO2 evolution test” was used to analyze the ultimate biodegradability of 10 commonly used surfactants and liquid detergents of different brands and categories on the market, to examine their impact on the environment. This method simplified the experimental device and was easy to operate. In addition, it did not require to collect carbon dioxide, so the experimental data would not be able to deviate due to incomplete carbon dioxide capture. The error analysis of the experimental results shows that the method has stable experimental data and high repeatability. The results of ultimate biodegradability show that, the degradation rate of several common surfactants is above 60%, which meets the environmental requirements. Except for LAS, the rest are all more than 80%, indicative of excellent ultimate biodegradability. The degradation rate of some detergent products on the market is also greater than 80%, indicative of excellent ultimate biodegradability.

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    丹参水溶性提取物丹参酚酸B的制备及应用
    Study on the preparation and application of salvianolic acid B, a water-soluble extract of Salvia miltiorrhiza
    陈萍萍,许全升,赵丽娜,张晓霞
    2022 (10):  1100-1106.  doi: 10.3969/j.issn.1001-1803.2022.10.010
    摘要 ( 235 )   HTML ( 13 )   PDF(1261KB) ( 248 )  

    探讨丹参水溶性提取物丹参酚酸B的制备及其生物转化应用研究。以丹参酚酸B的出膏率和提取率为评价指标,比较丹参水溶性提取法包括水煎煮回流法、超声提取法、渗漉提取法,采用高效液相色谱(HPLC)法测定。研究发现,常规水煎煮回流法中丹参酚酸B提取率最高可达72.59%,远高于超声提取法的63.72%和渗漉提取法的65.69% (P<0.05)。丹参酚酸B的生物转化应用结果显示,100 g丹参酚酸B可以制备出14.2 g丹参素(纯度≥95%)和35.8 g Prewalskinic acid A(纯度≥91%),转化效率高。对丹参水溶性提取物丹参酚酸B的制备工艺进行了相关研究,获得了简便、高效、科学的工艺路线,该研究为丹参的进一步开发和实际应用奠定了理论和实践基础。

    The purpose was to study the preparation and biotransformation application of salvianolic acid B, a water-soluble extract of Salvia miltiorrhiza. The extraction rate and extraction rate of salvianolic acid B were used as evaluation indicators to compare the water-soluble extraction methods of Salvia miltiorrhiza, including water decoction reflux method, ultrasonic extraction method, percolation method, etc., which were determined by high performance liquid chromatography (HPLC). After repeated exploration and comparison, the study finds that the extraction rate of salvianolic acid B in the conventional water decoction reflux method is as high as 72.59%, which is much higher than of the ultrasonic extraction method of 63.72% and the percolation method of 65.69% (P<0.05). In the application of biotransformation of salvianolic acid B, the study finds that 100 g of salvianolic acid B can yield 14.2 g of Danshensu (purity≥95%) and 35.8 g of Prewalskinic acid A (purity≥91%), which indicates that the biotransformation is very successful. In this study, we have conducted related research on the preparation process of salvianolic acid B, a water-soluble extract of Salvia miltiorrhiza, obtained a simple, efficient and scientific process route, and studied its biotransformation application, which found a high conversion efficiency of salvianolic acid B into Przewalskinic acid A and Danshensu. This research lays a theoretical and practical foundation for the further development and practical application of Salvia miltiorrhiza.

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    基于MALDI-TOF MS技术对面膜中污染日勾维多细菌源菌的鉴定分析
    Identification and analysis of Pluralibacter gergoviae in facial masks based on MALDI-TOF MS
    谭慧敏,王涛,朱斌,零文超,樊兰艳
    2022 (10):  1107-1112.  doi: 10.3969/j.issn.1001-1803.2022.10.011
    摘要 ( 211 )   HTML ( 3 )   PDF(1571KB) ( 241 )  

    对149批面膜产品进行微生物检验,其中4批菌落总数不符合规定。对不合格样品中分离纯化的菌落用MALDI-TOF MS、16S rDNA测序比对、VITEK 2生化试验3种方法进行鉴定,结果均为日勾维多细菌源菌(Pluralibacter gergoviae);检出菌与日勾维多细菌源菌标准菌株CICC 24132和一株食品中检出的日勾维多细菌源菌共6株菌在MALDI Biotyper 3及VITEK 2生化反应基础上进行分析分型,经MALDI Biotyper 3对6株菌的蛋白图谱进行聚类分析,来源于面膜中的4株菌亲缘关系比较近;经对比VITEK 2生化试验发现,6株日勾维多细菌源菌生化反应存在差异,其中来源于同一生产厂家的3批面膜检出菌生化反应基本相同。结果表明,MALDI-TOF MS快速鉴定结果可信;经MALDI Biotyper 3聚类分析及生化反应的结果分析,可将4株面膜中分离的日勾维多细菌源菌分成两个亚型,从同一厂家3批不合格样品中检出的污染菌具有高度同源性。

    A total of 149 batches of facial mask products were tested for microorganism, and 4 batches did not meet the requirements. The bacterial colonies of these 4 batches of facial mask products were purified, and identified by MALDI-TOF MS, 16S rDNA sequencing and Vitek 2 biochemical test. The results show that they are all Pluralibacter gergoviae. In addition, Pluralibacter gergoviae CICC24132 and a food detected Pluralibacter gergoviae are analyzed with these four strains together by MALDI Biotyper 3 and VITEK 2. MALDI Biotyper 3 cluster analysis shows that the protein pattens detected in the four batches of facial mask are basically the same, with their relationship relatively close to each other, but far from the other 2 strains. Biochemical tests of VITEK 2 show that there are differences in the biochemical reactions of 6 strains of Pluralibacter gergoviae, among which the bacteria detected in 3 batches of masks from the same manufacturer are basically the same. The results suggest that the rapid identification results of MALDI-TOF MS are reliable. MALDI Biotyper 3 cluster analysis and biochemical reaction results show that the 4 strains of Pluralibacter gergoviae isolated from facial masks can be divided into two subtypes, and the contaminated bacteria detected from three batches of unqualified samples from the same manufacturer have high homology.

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    专论与综述
    我国化妆品智慧审评技术要点分析
    Technical key points of intelligent evaluation of cosmetics in China
    苏哲,胡康,吕冰峰,塔娜,王钢力,路勇
    2022 (10):  1113-1120.  doi: 10.3969/j.issn.1001-1803.2022.10.012
    摘要 ( 252 )   HTML ( 13 )   PDF(1118KB) ( 423 )  

    为落实《化妆品监督管理条例》,国家药品监督管理局构建了全新的化妆品法规和技术体系,并组织建设化妆品注册备案信息服务平台,中国食品药品检定研究院积极开展了化妆品智慧审评相关工作。论文在此基础上,以《化妆品监督管理条例》及其配套法规为依据,围绕电子资料内容和技术审评工作要求,对能够通过系统完成一定自动化判定和提示的审评要点进行梳理,对具体实现路径、需整合数据库、判断逻辑等进行分析,并讨论了在技术审评和监管工作中的应用。目前,已成功建立起一系列智慧审评要点,覆盖产品配方和原料使用、产品检验报告、产品标签样稿、产品执行的标准、安全评估报告等审评内容,并研究了功效宣称评价依据摘要的规范化填报和自动形式审核,为化妆品智慧审评和智慧监管工作提供了技术支撑。

    In order to implement the Regulations on the Supervision and Administration of Cosmetics, the National Medical Products Administration has established new regulations and technical systems and organized the construction of a cosmetics registration and filing information service platform. The National Institutes for Food and Drug Control has carried out research on the intelligent evaluation of cosmetics. In this study, based on the Regulations on the Supervision and Administration of Cosmetics and its supporting regulations, the contents of the registration or filing documents and the concerns in technical evaluation work, the researchers summarized the key points that could be automatically detected and reviewed by the IT system, analyzed the technical path, databases to be integrated, and logic rules, and discussed the possible application in technical evaluation and supervision. So far, a series of key points for intelligent evaluation of cosmetics have been established, covering product formula and ingredient use, product test reports, product label, product implementation standard and safety evaluation report, and a standardized filling and automatic formal examination of the abstract of efficacy claim evaluation has also been developed. This work will provide technical support for intelligent evaluation and supervision of cosmetics in China.

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    除臭剂与除臭化妆品的研究进展
    Research progress on deodorants and deodorizing cosmetics
    崔小倩,赵梦恬,陈彦君,曹高
    2022 (10):  1121-1127.  doi: 10.3969/j.issn.1001-1803.2022.10.013
    摘要 ( 295 )   HTML ( 17 )   PDF(1153KB) ( 399 )  

    随着《化妆品监督管理条例》的颁布与实施,除臭化妆品变为普通化妆品,不再属于特殊化妆品管理范围。人们对除臭化妆品日益增长的需求使一系列新型的除臭化妆品与除臭剂问世,天然温和、安全低敏成为了开发这类化妆品追求的目标。本文综述了体臭产生的机理;总结了除臭化妆品控制体臭的方法;着重介绍了除臭日化原料的最新研究应用进展;并对除臭化妆品领域的产品开发提出建议,指出标本兼治、回归天然、注重功效将是除臭化妆品领域研究的方向,以期为市场开发安全高效的除臭化妆品提供参考。

    After the implementation of the Regulations on the Supervision and Administration of Cosmetics, deodorizing cosmetics are no longer special cosmetics, but ordinary cosmetics. In recent years, the increasing demand for deodorizing cosmetics has led to the emergence of a series of new deodorizing cosmetics and deodorants. Additionally, not only efficacy, but natural mildness, safety and low sensitivity have become the key to the development of this kind of cosmetics. In this review, the mechanism of body odor and the four methods of controlling body odor by deodorizing cosmetics are summarized. Then, the latest research and application progress of deodorants in cosmetics are emphatically introduced. In general, in order to develop safe and efficient deodorizing cosmetics, cosmetic producers and scientists should treat both the symptoms and root causes of body odor, as well as focus on natural deodorants and their efficacy.

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    分析与检测
    超高效液相色谱法快速测定化妆品中23种防腐剂
    Rapid determination of 23 preservatives in cosmetics by ultra performance liquid chromatography
    张伟清,刘慧锦,王海燕,孙磊
    2022 (10):  1128-1134.  doi: 10.3969/j.issn.1001-1803.2022.10.014
    摘要 ( 227 )   HTML ( 14 )   PDF(1090KB) ( 265 )  

    采用超高效液相色谱法,建立同时测定化妆品中23种防腐剂的快速分析方法。样品用甲醇提取,经CAPCELL CORE C18(2.1 mm×150 mm,2.7 μm)色谱柱分离,流动相为0.1%磷酸-乙腈,梯度洗脱,流速为0.4 mL/min,检测波长为280,254及230 nm。分析结果表明,该方法的方法学验证结果良好,分离效果好,分析时间短,操作简便,流动相组成简单,可用于日常化妆品中防腐剂的快速检测。

    A rapid analytical method for the simultaneous determination of 23 preservatives in cosmetics was established by ultra-high performance liquid chromatography (UPLC). The sample was extracted with methanol and separated by CAPCELL CORE C18 column (2.1 mm×150 mm, 2.7 μm) chromatographic column separation using 0.1% phosphoric acid acetonitrile as the mobile phase with gradient elution. The flow rate was 0.4 mL/min, and the detection wavelength was 280, 254 and 230 nm. The results show that the method has good methodological validation, good separation effect, short analysis time, simple operation and simple composition of mobile phase, which can be used for rapid detection of preservatives in daily cosmetics.

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    高效液相色谱法测定醇醚羧酸盐中羟基乙酸、一氯乙酸和二氯乙酸的含量
    Determination of glycolic acid, monochloroacetic acid and dichloroacetic acid in alkylpolyethoxy carboxylate by HPLC
    张军,杨秀全,周媛,白亮,吴志宇
    2022 (10):  1135-1139.  doi: 10.3969/j.issn.1001-1803.2022.10.015
    摘要 ( 645 )   HTML ( 9 )   PDF(1018KB) ( 336 )  

    建立了一种高效液相色谱法测定醇醚羧酸盐产品中羟基乙酸、一氯乙酸和二氯乙酸含量的方法。样品经流动相溶解后直接进样分析,采用具有反相和阴离子交换两种分离模式的Acclaim Trinity P1色谱柱(3.0 mm×150 mm,3 μm)进行分离,以体积分数为10%乙腈-90%磷酸缓冲盐水溶液(10 mmol磷酸二氢钠,调节pH为5.0)洗脱,在紫外检测器210 nm波长下检测。经方法学验证,3种化合物在一定质量浓度范围内线性良好,相关系数均大于0.999,测定精密度、稳定性皆满足要求,测定平均回收率在96%~98%之间,相对标准偏差(RSD)皆小于3%。与GB/T 28193–2011《表面活性剂中氯乙酸(盐)残留量的测定》方法相比,该方法测定结果接近,但增加了羟基乙酸的测定,结果更加全面。与离子色谱法相比,该方法不受产品溶解性限制,可用于高碳链或水溶性不佳的产品体系,适用范围更宽。

    A method for determination of glycolic acid, monochloroacetic acid and dichloroacetic acid in alkylpolyethoxy carboxylate (AEC) by high performance liquid chromatography was established. The column was Acclaim Trinity P1 column (3.0 mm×150 mm, 3 μm) for separation and it was adapted gradient with 10% acetonitrile-90% phosphate buffered saline (10 mmol sodium dihydrogen phosphate, adjust pH to 5.0). A UV detector at 210 nm was used. The separation and determination of glycolic acid, monochloroacetic acid and dichloroacetic acid could be completed. The resolution of chromatographic peaks of the three compounds to be tested in the sample solution is good, and the peak area and concentration of the reference substance show good linear correlation, and the correlation coefficients are greater than 0.999. The stability and precision of the analysis meet the requirements of methodological investigation. The average recovery of three compounds is in the range from 96% to 98%, and the relative standard deviation (RSD) is less than 3%. Compared with the method of GB/T 28193—2011 (Determination of chloroacetic acid (chloroacetate) contents in surfactants), this method is not limited by product solubility, and can be used in product systems with long carbon chain or poor water solubility. Therefore, it has a wider scope of application, and it can provide references for AEC product quality control, production process upgrading and test method improvement.

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    高效液相色谱法同时测定祛痘类化妆品中的10种抗痤疮类化学成分及质谱确证
    Simultaneous determination of ten anti-acne compounds in anti-acne cosmetics by high performance liquid chromatography and verification by liquid chromatography-tandem mass spectrometry
    张珊珊,贾昌平
    2022 (10):  1140-1146.  doi: 10.3969/j.issn.1001-1803.2022.10.016
    摘要 ( 198 )   HTML ( 13 )   PDF(1115KB) ( 245 )  

    建立了同时检测祛痘类化妆品中的10种抗痤疮类成分(过氧苯甲酰、螺内酯、他卡西醇、他扎罗汀、阿维A、异维甲酸、维甲酸、依曲替酯、维胺酯、阿达帕林)的高效液相色谱-紫外筛查、定量方法及液相色谱-质谱定性确证方法。样品经甲醇提取后,经Agilent ZORBAX Extend-C18(4.6×250 mm,5 μm)色谱柱分离,以甲醇和乙酸水溶液为流动相梯度洗脱,PDA检测器多波长检测,外标法定量。结果表明,方法的回收率为80.8%~102.7%,相对标准偏差小于3.0%,10种抗痤疮类成分在各自的质量浓度范围内均呈良好的线性关系(相关系数均≥0.999 8),检出限为0.1~1.0 mg/kg。该方法具有前处理步骤简单、分析时间短、准确性好等特点,适用于化妆品中祛痘类化妆品中的10种抗痤疮类成分的定性筛查及含量测定。

    The purpose was to establish a method for the identification of ten anti-acne compounds (benzoyl peroxide, spironolactone, tacalcitol, tazarotene, acitretin, isotretinoin, tretino-in, etretinate, viaminate, adapalene) in anti-acne cosmetics by high performance liquid chromatography and verification by liquid chromatography-tandem mass spectrometry. The samples were extracted by ultrasonic machine with methanol. The separation was executed on an Agilent ZORBAX Extend-C18 column by a mobile phase consisting of 0.5% acetic acid (A), methanol (B), with the flow speed of 1.0 mL/min. The qualitative screening results were obtained through high performance liquid chromatography with PDA detector at multi-wavelength, the standard curve method was used for quantification, and the results of liquid chromatography tandem mass spectrometry were used for verification. The results show that under the conditions of this method, the recovery rate is 80.8%-102.7%, and the relative standard deviation is less than 3.0%. Ten anti-acne compounds obtain a good linear relationship within their respective mass concentration ranges, and the correlation coefficients are all greater than 0.999 8. The detection limits are 0.1-1.0 mg/kg. This method can be used exclusively and quickly to screen and confirm ten anti-acne compounds added in anti-acne cosmetics. It is mainly suitable for the simultaneous determination of ten anti-acne compounds in anti-acne cosmetics.

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