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    2020年, 第50卷, 第10期 刊出日期:2020-10-22 上一期    下一期
    基础研究
    新型清洁压裂液25-HP-21/NaSal胶束体系流变性研究
    Rheological properties of a novel clean fracturing fluid: the micellar system of 25-HP-21/NaSal
    崔秀,方波,许海涛
    2020 (10):  653-659.  doi: 10.3969/j.issn.1001-1803.2020.10.001
    摘要 ( 264 )   HTML ( 75 )   PDF(1673KB) ( 285 )  

    以芥酰胺丙基二甲胺、油酰胺丙基二甲胺、环氧氯丙烷为主要原料合成了新型不对称阳离子Gemini表面活性剂羟丙撑基(芥-油酰胺丙基二甲基氯化铵醋酸铵)(25-HP-21),将其与水杨酸钠(NaSal)进行复配研究了该黏弹性胶束体系的流变学性质、微流变学性质、耐温性能和携砂性能,并采用1H NMR表征了NaSal对25-HP-21胶束聚集形态的影响。研究结果表明:在体系中25-HP-21含量固定为2%的情况下改变NaSal的含量,得出25-HP-21/NaSal胶束体系的优化配比为5∶1(w/w);另外,在固定25-HP-21/NaSal的质量比为5∶1的情况下改变表面活性剂的浓度,则发现3.6%的25-HP-21/NaSal胶束体系具有更优的黏弹性、更显著的剪切变稀性和触变性以及较优的耐温性能和携砂性能;体系的1H NMR谱图结果表明NaSal的加入有利于促进蠕虫状胶束的形成,表面活性剂分子排列更加紧密。该胶束体系配方简单、性质优异,有望丰富新型清洁压裂液。

    Erucamidopropyl dimethylamine, oleamidopropyl dimethylamine and epichlorohydrin were used as the main raw materials to synthesize a novel asymmetric cationic Gemini surfactant, i.e. hydroxypropylene(erucamido-oleamido propyl dimethyl ammonium) chloride acetate (25-HP-21). Then 25-HP-21 was mixed with sodium salicylate (NaSal) to obtain a viscoelastic micellar system. The rheological properties, microrheological properties, temperature-resistance and sand-carrying properties of the micellar system were studied. The effects of NaSal on the aggregate morphology of 25-HP-21 micelles was characterized by1H NMR. The results showed that, when the content of 25-HP-21 in the mixed system was fixed to 2%, the optimized ratio of 25-HP-21/NaSal for this micellar system was 5∶1 (w/w). In addition, when the mass ratio of 25-HP-21/NaSal was fixed to 5∶1, the micellar system of 3.6% 25-HP-21/NaSal showed better viscoelasticity, temperature-resistance and sand-carrying properties and more significant shear thinning and thixotropy. The1H NMR spectrum of the system showed that the addition of NaSal was beneficial to the formation of worm-like micelles, and the arrangement of surfactant molecules were more compact. This micellar system had a simple formula and excellent properties, which was expected to enrich the family of novel clean fracturing fluids.

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    科技讲座
    两亲聚合物设计合成及其增效体系研究(Ⅹ)—— 油藏适应性
    Study on the design and synthesis of amphiphilic polymers and their synergistic systems (X) Reservoir adaptability
    康万利,范宇恒,杨红斌,Bauyrzhan Sarsenbekuly
    2020 (10):  660-668.  doi: 10.3969/j.issn.1001-1803.2020.10.002
    摘要 ( 195 )   HTML ( 11 )   PDF(1014KB) ( 405 )  

    两亲聚合物以其良好的耐温、抗盐以及乳化原油特性,在油田矿场应用中取得了一定的增油效果。为进一步深入认识两亲聚合物在油田中的应用效果,本文基于国内外的矿场应用实例以及两亲聚合物本身的物化性能,从油藏类型(稠油油藏,稀油油藏)、油藏温度以及油藏矿化度等方面综述了两亲聚合物及其增效体系与油藏的适应性。最后基于矿场应用条件,指出了未来两亲聚合物及其增效体系的发展趋势。

    Amphiphilic polymers have achieved a certain oil-increasing effect in oilfield applications due to their good temperature resistance, salt resistance and crude-oil-emulsifying properties. In order to further understand the application effects of amphiphilic polymers in oilfields, the application examples in domestic and foreign oilfields and the physical and chemical properties of amphiphilic polymers have been introduced. The adaptability of the amphiphilic polymers and their synergistic systems to the reservoir has been reviewed in terms of reservoir type (heavy oil reservoir or thin oil reservoir), reservoir temperature and reservoir salinity. Finally, based on the application conditions, the development trend of the amphiphilic polymers and their synergistic systems in the future has been pointed out.

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    开发与应用
    含硒表面活性剂n-庚基-硒-n-辛基硫酸酯钠的合成与性质
    Synthesis and properties of sodium n-heptylselanyloctyl sulfate
    刘德琼,张永民,樊晔,刘雪锋,方银军
    2020 (10):  669-675.  doi: 10.3969/j.issn.1001-1803.2020.10.003
    摘要 ( 256 )   HTML ( 8 )   PDF(1563KB) ( 318 )  

    含硒表面活性剂的分子疏水尾链中嵌插有二价硒醚基团(-Se-),是具有Redox-开关响应的功能表面活性剂。为进一步丰富含硒表面活性剂的研究,设计并合成了一种含硒阴离子表面活性剂n-庚基-硒-n-辛基硫酸酯钠(C7SeC8SO4Na),在C7SeC8SO4Na水溶性、降低气/液和液/液界面张力、泡沫和乳化等性质研究的基础上,考察了C7SeC8SO4Na的氧化(H2O2)还原(Na2SO3)可逆响应行为。结果表明,C7SeC8SO4Na的Krafft温度为(21.7±0.3) ℃,其cmc值为7.3×10-4 mol/L(30 ℃,吊环法);在H2O2的作用下,C7SeC8SO4Na分子中的-Se-基团可以被氧化成四价硒亚砜基团(-SeO-)最终得到C7SeOC8SO4Na;与C7SeC8SO4Na相比,C7SeOC8SO4Na的水溶性更好,但是降低表(界)面张力、泡沫和乳化等性能明显更差;在Na2SO3的作用下,C7SeOC8SO4Na被还原成C7SeC8SO4Na,其降低表(界)面张力、泡沫和乳化等性能得以复原。

    The selenium-containing surfactants are functional surfactants with a redox-switchable divalent selenide group (-Se-) embedded in the hydrophobic tail. In order to further enrich the research of Se-containing surfactants, an anionic surfactant of sodium n-heptylselanyloctyl sulfate (C7SeC8SO4Na) was synthesized. Its water solubility, reduction of gas-liquid and liquid-liquid interfacial tensions, foaming properties and emulsifying properties were studied. The reversible redox-response behavior of C7SeC8SO4Na was investigated. The results showed that, the Krafft temperature of C7SeC8SO4Na was (21.7±0.3) ℃, and its critical micelle concentration was 7.3×10-4 mol/L (30 ℃, ring method). C7SeC8SO4Na was transformed into C7SeOC8SO4Na after oxidation with H2O2 because the selenide group in C7SeC8SO4Na was oxidized to the selenoxide group. Compared with C7SeC8SO4Na, C7SeOC8SO4Na had better water solubility, but the abilities of reducing surface and/or interfacial tensions, foaming and emulsification were obviously worse. After reduction with Na2SO3, C7SeOC8SO4Na was restored to its reduced form (C7SeC8SO4Na), and then the abilities of reducing surface and/or interfacial tensions, foaming and emulsification were recovered.

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    脂肪醇醚琥珀酸酯盐的性能研究
    Study on the properties of salts of fatty alcohol polyoxyethylene ether succinates
    吴志芳,李运玲
    2020 (10):  676-680.  doi: 10.3969/j.issn.1001-1803.2020.10.004
    摘要 ( 275 )   HTML ( 11 )   PDF(1233KB) ( 403 )  

    研究了不同环氧乙烷(EO)数的新型脂肪醇醚琥珀酸酯盐表面活性剂(AEnCE-Na,n=3,5,7,9)的平衡表面张力、动态表面张力、接触角,及包括润湿性、乳化性、泡沫性和去污性在内的应用性能。结果表明:AE3CE-Na不仅在表面活性方面降低表面张力的效率和能力最强,而且在石蜡膜上的润湿性也最好。不同EO加合数的AEnCE-Na整体的扩散速率均较快。在应用性能方面,AE3CE-Na的润湿性、乳化性(包括液体石蜡和大豆油)和发泡性最佳,AE9CE-Na的去污性和稳泡性最佳。

    A series of novel surfactants, i.e. salts of fatty alcohol polyoxyethylene ether succinates with different ethylene oxide (EO) numbers (AEnCE-Na, n=3, 5, 7, 9), were studied by measurement of equilibrium surface tension, dynamic surface tension, contact angle as well as the evaluation of application performance in wetting, emulsifying, foaming and detergency. The results showed that, AE3CE-Na not only exhibited the highest efficiency and ability to reduce the surface tension of solutions, but also showed the best wettability on the paraffin film. The diffusion rate of AEnCE-Na with different EO numbers were all fast. In terms of application performance, AE3CE-Na showed the best wetting, emulsifying (including liquid paraffin and soybean oil) and foaming properties, while AE9CE-Na showed the best detergency and foam stability.

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    N-酰基氨基酸型表面活性剂与离子液体表面活性剂复配体系流变性研究
    Rheology of the mixed aqueous systems of N-acyl amino acid surfactant and ionic liquid surfactant
    惠蒙蒙,白亚榕,杨许召,张晨龙,王军
    2020 (10):  681-686.  doi: 10.3969/j.issn.1001-1803.2020.10.005
    摘要 ( 314 )   HTML ( 18 )   PDF(1331KB) ( 380 )  

    通过表面张力和流变性的测定研究了离子液体表面活性剂1-十四烷基-3-甲基咪唑溴盐([C14Mim][Br])与月桂酰基肌氨酸钠(SLS)、月桂酰基谷氨酸钠(SLGLU)和月桂酰基甘氨酸钠(SLG) 3种N-酰基氨基酸型表面活性剂之间的相互作用和不同复配比例时混合体系的流变特征。除SLG外,SLS和SLGLU与不同摩尔分数(x)的[C14Mim][Br]具有良好的复配稳定性。SLS、SLGLU分别与[C14Mim][Br]复配后降低水溶液表面张力能力具有协同增效作用,SLGLU与[C14Mim][Br]的协同增效作用大于SLS与[C14Mim][Br],其最佳复配x分别为0.7和0.5。SLS与[C14Mim][Br]和SLGLU与[C14Mim][Br]两种混合体系在大部分复配比例时都没有触变环,只有x=0.4~0.5的SLS+[C14Mim][Br]混合溶液和x=0.7的SLGLU+[C14Mim][Br]混合溶液呈现了触变环。两种复配体系都具有剪切变稀的特点,这可能与复配体系中形成了囊泡有关。除了x=0.5的SLS+[C14Mim][Br]混合溶液外,这两种复配体系的黏度基本不随剪切时间而改变,具有良好的耐剪切性。

    The interactions between an ionic liquid surfactant (1-tetradecyl-3-methylimidazolium bromine, [C14Mim][Br]) and three N-acyl amino acid surfactants (sodium lauroyl sarcosinate (SLS), sodium lauroyl glutamate (SLGLU) and sodium lauroyl glycinate (SLG)), and the rheology of the mixed aqueous systems of [C14Mim][Br]/SLS and [C14Mim][Br]/SLGLU with different mole fractions (x) of [C14Mim][Br] were studied by the determination of surface tension and rheology. Except SLG, the N-acyl amino acid surfactants under investigation showed a good formulation stability when mixed with [C14Mim][Br]. The surface tension of mixed solutions of [C14Mim][Br]/SLS and [C14Mim][Br]/SLGLU were both indicative of synergistic effect. The synergistic effect between [C14Mim][Br] and SLGLU was larger than that between [C14Mim][Br] and SLS, and the optimum x were 0.7 and 0.5, respectively. When a series of aqueous solutions of [C14Mim][Br]/SLS and [C14Mim][Br]/SLGLU were tested by thixotropy, there was no thixotropic loop for the mixed solutions except the solutions of [C14Mim][Br]/SLS at x=0.4-0.5 and the solution of [C14Mim][Br]/SLGLU at x=0.7. The two series of aqueous solutions showed the characteristics of shear thinning, which might be related to the formation of vesicles in the mixed systems. Except for the mixed solution of [C14Mim][Br]/SLS at x=0.5, no significant change was observed in the viscosity of the two mixed systems with shear time, indicative of good shear resistance.

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    改性壳寡糖中羧基含量对其吸湿保湿和抗氧化性能的影响
    Effects of carboxyl content in modified chitooligomer on moisture absorption-retention and anti-oxidant activities
    潘玙璠,张方东,卜鑫,裴继诚
    2020 (10):  687-692.  doi: 10.3969/j.issn.1001-1803.2020.10.006
    摘要 ( 282 )   HTML ( 13 )   PDF(1093KB) ( 331 )  

    采用漆酶/TEMPO/O2体系(TEMPO用量控制在1%,2%,4%和8%)氧化壳寡糖(COS)制备得到改性壳寡糖(MC),利用电导滴定和低场核磁共振波谱(LF-NMR)分析产物中羧基含量及水的存在形态,并检测了吸湿保湿性和抗氧化性能。结果表明,MC中羧基含量随着TEMPO用量增加而增多,MC-8中羧基含量最高达2.82%;随着羧基含量的增加,MC分子内结合水数量先增加后减小,吸湿保湿能力也呈现相同变化趋势,MC-2在饱和硫酸铵和饱和碳酸钾溶液中60 h的吸湿率最高达63.14%和20.26%,24 h的保湿率为4.71%;羧基含量的增加有利于提高产物的抗氧化性能,MC-8在0.5 g/L质量浓度下ABTS自由基清除率为85.47%。改性壳寡糖的研究在化妆品领域具有潜在的应用价值。

    Modified chitooligomer (MC) was prepared by oxidation of chitooligomer (COS) using laccase/TEMPO/O2 system (TEMPO dosage was controlled at 1%, 2%, 4% and 8%). The carboxyl content and water existing forms in products were analyzed by conductometric titration and low-field nuclear magnetic resonance (LF-NMR), and the moisture absorption-retention activity and anti-oxidant activity were detected. The results show that the carboxyl content in MC increases with the TEMPO usage, and the carboxyl content in MC-8 is as high as 2.82%. With the increase of carboxyl content, the amount of bound water in MC increases at first and then decreases, and the moisture absorption-retention capacity shows the same trend. The moisture absorption rate of MC-2 in saturated ammonium sulfate and saturated potassium carbonate solution for 60 h is up to 63.14% and 20.26%, respectively. The moisture retention rate for 24 h is 4.71%. The increase of carboxyl content is beneficial to improve the anti-oxidant activity of the product, and the ABTS radical scavenging rate of MC-8 at the mass concentration of 0.5 g/L is 85.47%. The study indicates that MC has potential application value in the field of cosmetics.

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    低共熔溶剂中乙酸异戊酯的绿色合成
    Green synthesis of isoamyl acetate in deep eutectic solvent
    王英磊,李文欢,耿孝彬,李津,谢英男
    2020 (10):  693-697.  doi: 10.3969/j.issn.1001-1803.2020.10.007
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    以冰乙酸和异戊醇为原料,采用低共熔溶剂氯化胆碱-氯化锌作为催化剂合成乙酸异戊酯,目标产物经折射率测定,红外光谱和核磁共振氢谱表征。考察了反应物配比、低共熔溶剂用量、反应温度、反应时间等因素对乙酸异戊酯合成的影响。结果表明,较佳合成条件为:酸醇摩尔比1.2∶1,氯化胆碱-氯化锌用量2.0 g,反应温度110 ℃,反应时间3.0 h,此时,乙酸异戊酯的收率可达93%。同时,氯化胆碱-氯化锌回收利用5次产品收率仍然可达85%。

    Isoamyl acetate was synthesized by using acetic acid and isoamyl alcohol as raw materials, and deep eutectic solvent choline chloride-zinc chloride as catalyst. The target product was measured by refractive index, and characterized by FT-IR and1H NMR. The effects of reactant ratio, deep eutectic solvent dosage, reaction temperature and reaction time on the yield of isoamyl acetate were studied. Results showed that the yield of isoamyl acetate can reach 93% when the molar ratio of acetic acid to isoamyl alcohol is 1.2∶1, the dosage of choline chloride-zinc chloride is 2.0 g, the reaction temperature is 110 ℃ and the reaction time is 3.0 h. In addition, choline chloride-zinc chloride was recovered and recycled for five times, and the product yield could still reach 85%.

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    化妆品微生物污染状况及其防腐剂使用情况分析
    Analysis of microbial contamination and preservative use in cosmetics
    张静,刘绪平,易路遥,张春华,章瑛
    2020 (10):  698-703.  doi: 10.3969/j.issn.1001-1803.2020.10.008
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    通过对化妆品的微生物污染状况及其防腐剂使用情况进行分析,评价其防腐体系对微生物污染的控制能力。按《化妆品安全技术规范》(2015年版)(以下简称《规范》)对38批次市售化妆品的微生物和防腐剂进行检测,对检出情况进行整理汇总;参照《中国药典》(2015年版)四部通则1121抑菌效力检查法进行抑菌性实验。检验结果显示3批次检出微生物指标不合格,不符合《规范》的要求,检出污染菌经鉴定有豕链球菌、玫瑰色考克氏菌、成团泛菌;防腐剂种类及使用浓度均在《规范》要求范围内,7批使用4-羟基苯甲酸酯类,3批使用苯氧乙醇,1批使用甲基异噻唑啉酮,23批使用复合防腐剂;38批次化妆品均通过抑菌效力挑战实验。结果表明:化妆品微生物指标控制不能完全依赖于防腐剂,生产企业应严格控制防腐剂的使用范围及用量,并应对生产工艺和生产环境进行控制,加强生产环节中的微生物控制,提高产品质量。

    The microbial contamination of cosmetics and the use of preservatives were analyzed, and the control ability of the preservative system to microbial contamination was evaluated. According to “Safety and Technical Standards for Cosmetic” (2015th Edition) (hereinafter referred to as “Standards”), 38 batches of microorganisms and preservatives of commercial cosmetics were detected, and the detection conditions were summarized; the bacteriostatic test was carried out according to the general rule 1121 of the fourth part of Chinese Pharmacopoeia (2015th Edition). The results show that the microbiological indexes of three batches are unqualified, which does not meet the requirements of the “Standards”. The contaminating bacteria are identified as Streptococcus porcinus, Kocuria rosea, and Pantoea agglomerans. The type and concentration of preservatives are within the requirements of the “Standards”. 7 batches use 4-hydroxybenzoates, 3 batches use phenoxyethanol,1 batch use methyl isothiazolinone, and 23 batches use composite preservative. 38 batches of cosmetics all pass the antibacterial efficacy challenge experiment. The results show that the control of microbiological index in cosmetics cannot be completely dependent on preservatives. Manufacturers should strictly control the scope and dosage of preservatives, control the production process and production environment, strengthen the microbiological control in the production process, and improve the product quality.

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    双光子成像技术在痤疮丙酸杆菌引起痤疮表皮炎症中的应用
    Application of two-photon imaging technology in epidermal inflammation of acnes caused by Propionibacterium acnes
    贺改英,唐靖惠,孙娅楠,马淑骅,杨伟峰,王毅
    2020 (10):  704-710.  doi: 10.3969/j.issn.1001-1803.2020.10.009
    摘要 ( 234 )   HTML ( 7 )   PDF(2789KB) ( 363 )  

    通过双光子激发荧光(Two-Photon Excitation Fluorescence,TPEF)成像技术和其他方法检测痤疮丙酸杆菌(Propionibacterium acnes,P.acnes)引起痤疮表皮炎症的变化。取对数生长期的P.acnes注射至小鼠耳部,通过TPEF成像技术检测表皮厚度、颗粒层、棘层和基底层细胞的变化,同时通过耳朵厚度测量和HE染色方法对耳朵和表皮厚度进行检测。TPEF成像技术发现P.acnes感染耳朵引起表皮厚度显著增加,颗粒层细胞内部分子发生重排,棘层和基底层细胞形态改变。耳朵厚度测量和HE染色发现P.acnes感染后耳朵和表皮厚度增厚。

    Changes of epidermal inflammation caused by Propionibacterium acnesP.acnes) were detected by Two-Photon Excitation Fluorescence (TPEF) imaging technology and other methods. P.acnes in the logarithmic growth phase were injected into the ears of mice, and the changes in epidermal thickness, stratum granulosum, stratum spinosum and stratum basale cells were studied by TPEF imaging technology. Thickness of ear and epidermis were detected by ear thickness measurement and HE staining method. TPEF imaging technology found that the epidermis thickness was increased significantly, the molecules in granular cells were rearranged, and the morphology of stratum spinosum and stratum basale cells was changed after P.acnes infection. Ear thickness measurement and HE staining revealed that the ear and epidermis infected by P.acnes became thicker.

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    活性炭负载磷钨酸季铵盐催化合成罗汉柏木烷酮
    Synthesis of thujopsanone catalyzed by activated carbon supported quaternary ammonium phosphotungstate
    张胜,朱凯
    2020 (10):  711-716.  doi: 10.3969/j.issn.1001-1803.2020.10.010
    摘要 ( 233 )   HTML ( 6 )   PDF(1599KB) ( 436 )  

    以磷钨酸、H2O2和十六烷基三甲基氯化铵为原料制备磷钨酸季铵盐催化剂(QAP),并将磷钨酸季铵盐负载在活性炭上制备活性炭负载磷钨酸季铵盐催化剂,通过FT-IR、XRD、SEM等对催化剂进行表征,将其用作合成罗汉柏木烷酮的催化剂。考察了反应条件对氧化反应的影响,得到最佳工艺条件为:磷钨酸季铵盐负载量为30%,反应温度为70 ℃,n(H2O2)∶n(罗汉柏木烯)=1.8∶1,反应时间为6 h,催化剂用量为8%(以罗汉柏木烯质量计,下同)。在此条件下,罗汉柏木烷酮的收率为65.7%,罗汉柏木烯的转化率为90.9%,罗汉柏木烷酮的选择性为72.3%,催化剂可循环使用3次。

    A catalyst, namely quaternary ammonium phosphotungstate, was prepared by using phosphotungstic acid, H2O2 and cetyltrimethylammonium chloride as raw materials. Then, activated carbon was used to support the catalyst to form an activated carbon-supported phosphotungstic acid quaternary ammonium salt catalyst. The structure of the catalyst was characterized by FT-IR, XRD and SEM. It was used as a catalyst for the synthesis of thujopsanone. The effects of reaction conditions on the oxidation were studied. The optimized reaction was obtained under the conditions as follows: quaternary ammonium phosphotungstate loading was 30%; the reaction temperature was 70 ℃; the molar ratio of raw materals was n(H2O2)∶n(thujopsene) of 1.8∶1; the reaction time was 6 h; the catalyst was added in the amount corresponding to 8% of thujopsene. Meanwhile, the yield of thujopsanone, the conversion of thujopsene and the selectivity to thujopsanone were 65.7%, 90.9% and 72.3%, respectively, and the catalyst could be recycled for three times.

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    专论与综述
    脂质对皮肤状态的影响及对相关化妆品研发的指导
    Effects of lipids on skin condition and guidance on the development of related cosmetics
    胡雪情,周明月,杨曼丽,陈风,何聪芬,贾焱
    2020 (10):  717-724.  doi: 10.3969/j.issn.1001-1803.2020.10.011
    摘要 ( 495 )   HTML ( 24 )   PDF(854KB) ( 1017 )  

    皮肤脂质通过不同的机制显著影响皮肤状态,进一步的研究需要使用脂质组学—— 一种更强大高通量、高分辨率的脂质分析工具,全面鉴定数千种皮肤脂质成分。通过对脂质结构和功能的验证,以研究单个脂质组分对皮肤状态的影响。文章从物理化学、生物化学、微生态3个功能方面综述皮肤脂质对皮肤状态的作用及其机制,并对脂质组学数据如何促进皮肤脂质对皮肤状态影响机制的研究进行阐述,指导相关化妆品的研发。

    Skin lipids dramatically influence the skin condition by different mechanisms. Further research needs the use of lipidomics which has more powerful analytical ability and high-throughput manner, to identify skin lipid components into individual species. The validation of structure and function of lipids was operated to study the process that individual lipid species was involved in. The effects and mechanisms of skin lipids on skin conditions were reviewed from three aspects of functions in physical chemistry, biochemistry and microecology. Additionally, the integration of lipidomics data with other omics strategies could develop the power to study the mechanism of skin lipids influencing skin condition, which could guide the relevant research and development of cosmetics.

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    分析与检测
    气相色谱-串联质谱法测定化妆品中24种致敏芳香化合物
    Determination of 24 fragrance allergens in cosmetics by gas chromatography-tandem mass spectrometry
    龙培,郑琳,高佳男,吴一鑫,许佳明,任飞,肖道清
    2020 (10):  725-730.  doi: 10.3969/j.issn.1001-1803.2020.10.012
    摘要 ( 245 )   HTML ( 12 )   PDF(879KB) ( 312 )  

    建立了化妆品中24种致敏芳香化合物的气相色谱-串联质谱(GC-MS/MS)分析方法。化妆品试样经甲醇超声提取,加入无水硫酸钠脱水,经离心过滤后,采用GC-MS/MS进行分析,外标法定量。结果显示,24种致敏芳香化合物的检出限为1~28 μg/L,线性范围内相关系数均大于0.995。选取了香水、保湿水、洁面膏3种类型的化妆品作为加标基质来验证方法的准确度,24种致敏芳香化合物的加标回收率为70.1%~119.6%,相对标准偏差为0.8%~7.0%(n=6)。该方法准确、灵敏,且前处理简单、快速,适用于化妆品中24种致敏芳香化合物的测定。

    A gas chromatography-tandem mass spectrometry (GC-MS/MS) method was developed for the simultaneous determination of 24 fragrance allergens in cosmetics. After ultrasonically extracted by methanol and dehydrated by adding anhydrous sodium sulfate, the cosmetics samples were centrifuged, filtered and analyzed by GC-MS/MS with external standard method. The limits of detection of 24 fragrance allergens range from 1 to 28 μg/L, and the correlation coefficients in the linear range were all greater than 0.995. Three types of cosmetics, including perfume, moisturizing water and cleansing cream, were selected to verify the accuracy of the method. The average spiked recoveries range from 70.1% to 119.6%, and the relative standard deviations (RSD) varies from 0.8% to 7.0% (n=6). The method is simple, rapid, accurate and sensitive, and suitable for the determination of 24 fragrance allergens in cosmetics.

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    SPE-GC-MS检测儿童驱蚊扣中8种菊酯类物质
    Determination of eight pyrethroids in children’s mosquito repellent products by SPE-GC-MS
    谭丽君,李欣
    2020 (10):  731-734.  doi: 10.3969/j.issn.1001-1803.2020.10.013
    摘要 ( 226 )   HTML ( 7 )   PDF(878KB) ( 337 )  

    建立检测市场上儿童驱蚊扣产品中菊酯类物质的气相色谱质谱方法,方法确定了甲醇为萃取溶剂,萃取液经HLB固相萃取小柱净化,以乙酸乙酯为洗脱溶剂,收集洗脱液,洗脱液经旋转蒸发浓缩后,用质谱检测器检测,确定每种菊酯类物质的特征离子,采用选择离子扫描(SIM),外标法定量。结果表明8种菊酯类化合物的质量浓度在0.05~1.0 mg/L范围内与其对应的峰面积成良好的线性关系,相关系数均不小于0.998,检出限为0.01~0.61 μg/L。3个加标水平样品的平均回收率为91.8%~119.2%,测定结果的相对标准偏差为0.94%~6.43%(n=5)。该方法前处理简便,线性和重复性良好,可用于驱蚊扣产品中菊酯类物质的检测。

    A gas chromatography-mass spectrometry (GC-MS) method was developed for the determination of pyrethroids residues in mosquito repellent products for children on the market. Methanol was identified as the extraction solvent. The extraction solution was purified by HLB solid phase extraction column. Ethyl acetate was used as the eluting solvent., After the eluate was concentrated by rotary evaporation, it was detected by a mass spectrometer to determine the characteristic ions of each pyrethroid substance, and quantified by selective ion scanning (SIM) and external standard method. The results show that there is a good linear relationship between the mass concentration of the eight pyrethroids and their corresponding peak area within the range of 0.05-1.0 mg/L,the correlation coefficients are not less than 0.998, and the detection limits are 0.01-0.61 μg/L. The average recoveries of the three spiked level samples are 91.8%-119.2%, and the relative standard deviations are 0.94%-6.43% (n=5). The method has the advantages of simple pretreatment, good linearity and repeatability, and can be used to detect pyrethroids in mosquito repellent products.

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