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    2019年, 第49卷, 第3期 刊出日期:2019-03-22 上一期    下一期
    基础研究
    头基含羟基的季铵盐双子表面活性剂的合成与性能
    Synthesis and properties of quaternary ammonium Gemini surfactants with hydroxyl in headgroups
    孙亚,潘华,韩富,周雅文,徐宝财
    2019 (3):  135-140.  doi: 10.3969/j.issn.1001-1803.2019.03.001
    摘要 ( 426 )   HTML ( 94 )   PDF(1136KB) ( 458 )  

    以溴代烷、二乙醇胺和1,4-二溴丁烷为原料,通过两步反应合成了一类头基含羟基的季铵盐双子表面活性剂亚丁基-1,4-双(烷基二羟乙基溴化铵)(m-4-m(OH),m=8,10,12,14),通过核磁共振氢谱( 1H NMR)和质谱(MS)对中间体和目标产物的结构进行表征。通过表面张力仪和电导率仪测定m-4-m(OH)在水溶液中的平衡表面张力(γcmc)和临界胶束浓度(cmc),并测定了其水溶液的乳化性能和泡沫性能。结果表明,烷基链越长,表面活性剂越容易自发形成胶束,14-4-14(OH)的cmc最低,可达0.48 mmol/L,γcmc为33.6 mN/m;头基中引入羟基可有效降低表面活性剂的cmc和γcmc;随着烷基链的增长,乳化性能越好;起泡性随着烷基链的增长呈先升后降的趋势。

    A series of quaternary ammonium Gemini surfactants with hydroxyl in headgroups, butylene-1,4-bis[di(2-hydroxyethyl)alkylammonium]dibromide (abbreviated as m-4-m(OH), where m=8, 10, 12, 14) were synthesized by two-step reactions with bromoalkane, diethanolamine and 1,4-dibromobutane. The structure of intermediate and final products were characterized by 1H NMR and mass spectrometry (MS). The surface tension (γcmc) and critical micelle concentration (cmc) of m-4-m(OH) in aqueous solution were determined by the surface tension and conductivity measurements. The emulsifying and foaming properties of m-4-m(OH) in aqueous solution were determined. It is shown that the aggregation of these Gemini surfactants are all spontaneous and the tendency of aggregation is increased with the alkyl chain length. The 14-4-14(OH) shows the lowest cmc (0.48 mmol/L) and γcmc (33.6 mN/m) among these Geminis. The cmc and γcmc of these surfactants in aqueous solution are significantly decreased due to the introduction of hydroxyethyl in the headgroup. The emulsifying property of m-4-m(OH) is better with the longer alkyl chain. The foaming property undergoes a maximum with increasing alkyl chain length.

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    科技讲座
    弱相互作用调控表面活性剂自组装(Ⅲ)——响应性表面活性剂
    Self-assembly of surfactants controlled by weak interactions(Ⅲ) Responsive surfactants
    于洋,郑利强,孙继超
    2019 (3):  141-149.  doi: 10.3969/j.issn.1001-1803.2019.03.002
    摘要 ( 519 )   HTML ( 17 )   PDF(1773KB) ( 499 )  

    天然的或合成的两亲分子(表面活性剂)可以自组装形成多尺度的聚集体结构,比如胶束、囊泡、液晶和纤维等。在表面活性剂中引入功能性基团,借助外界环境(比如光、温度、pH、CO2、磁等)的改变可以实现对表面活性剂的聚集方式的调控。本文主要介绍响应性表面活性剂的种类、结构以及环境刺激与响应性能之间的关系。

    Natural or synthetic amphiphiles such as surfactants can self-assemble to form multi-scale aggregate structures such as micelles, vesicles, liquid crystals, and fibers. The introduction of functional groups into surfactants can regulate the aggregation mode of surfactants with the help of changes in the external environment (such as light, temperature, pH, CO2, magnetism, etc.). In this paper, the category and structure of responsive surfactants are introduced, as well as the relationship between environmental stimuli and their responsive properties.

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    开发与应用
    聚醚和含氟酯共改性苯基含氢硅油的制备及消泡性能
    Preparation and defoaming performance of phenyl hydrogen-containing silicone oil co-modified with polyether and fluorine-containing ester
    郭睿,韩双,张瑶,王宁,高弯弯
    2019 (3):  150-155.  doi: 10.3969/j.issn.1001-1803.2019.03.003
    摘要 ( 410 )   HTML ( 11 )   PDF(1229KB) ( 418 )  

    以10-十一烯酸四氟丙酯(UATE)、聚醚(F-6)和苯基含氢硅油为原料,氯铂酸为催化剂,经硅氢加成反应合成了长链含氟烷基酯与聚醚共改性苯基含氢硅油(UAPFPS)。通过FT-IR和 1H NMR对UAPFPS的结构进行了表征,采用单因素试验对反应中各影响因素进行考察得到其较佳工艺参数为:反应温度110 ℃,反应时间5.5 h,n(Si-H) :n(C=C)=1:1.2,n(F-6) :n(UATE)=1:1,催化剂用量20 μg/g(相对于每克反应物)。在此条件下Si-H键转化率为95.30%。将UAPFPS、硅膏、乳化剂和增稠剂复配制得改性有机硅消泡剂,其性能测试结果表明,该消泡剂具有较好的消泡性、抑泡性与稳定性。

    10-Undecenoic acid tetrafluoropropyl ester (UATE), allyl polyether (F-6) and phenyl hydrogen-containing silicone oil were used as raw materials. Chloroplatinic acid was used as catalyst. The phenyl hydrogen-containing silicone oil co-modified with polyether and fluorine-containing ester (UAPFPS) was synthesized via hydrosilylation. The structure of UAPFPS was characterized by FT-IR and 1H NMR. The optimum parameters were obtained by single factor experiment: the reaction temperature was 110 ℃; the reaction time was 5.5 h; n(Si-H) :n(C=C)=1:1.2; n(F-6) :n(UATE)=1:1; the amount of catalyst is 20 μg/g (relative to each gram of reactant). Under this condition, the conversion of Si-H bonds was 95.30%. A modified silicone defoamer was prepared by compounding UAPFPS, silicone paste, emulsifiers and thickener. The results of performance test show that the defoamer has good defoaming properties, foam inhibition and stability.

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    琥珀酸酯磺酸盐的制备及性能
    Preparation and properties of a sulfosuccinate
    李伏益,葛赞,史立文,毛雪彬,雷小英,钟凯
    2019 (3):  156-161.  doi: 10.3969/j.issn.1001-1803.2019.03.004
    摘要 ( 513 )   HTML ( 10 )   PDF(1417KB) ( 865 )  

    用月桂酸与聚乙二醇-400进行酯化反应,酯化产物顺酐化再与亚硫酸钠进行磺化反应生成聚乙二醇脂肪酸酯琥珀酸酯磺酸盐。采用FT-IR对产品的结构进行表征,并对其乳液粒径、表面张力、接触角、发泡力、抑菌性能进行检测;将合成产物应用于皮革加脂处理,利用SEM观察皮革加脂前后的微观状态和形貌,并测试皮革力学性能。结果表明:制备聚乙二醇脂肪酸酯琥珀酸酯磺酸盐的乳液粒径为4.77 μm,Zeta电位为97.26 mV,泡沫体积为646 mL,临界胶束浓度(cmc)为8.59×10 -4 mol/L,接触角为63.1°;其对黑曲霉、铜绿假单胞菌和金色葡萄球菌较为敏感,最小抑菌浓度(MIC)分别为15,20和15 g/L;SEM结果表明,加脂后皮革的纤维束更细小,纤维间距变大;皮革抗张强度从22.07 MPa提高至28.24 MPa,断裂伸长率从64.7%降至36.4%。

    An esterification product was formed by reacting lauric acid with polyethylene glycol-400. The maleation of this ester was performed and the product was then sulfonated with sodium sulfite to form the disodium polyethylene glycol fatty acid ester sulfosuccinate. The structure of the product was characterized by FT-IR. The emulsion particle size, surface tension, contact angle, foaming power and antibacterial property were also tested. The microscopic state and morphology of leather before and after fat liquoring were compared by SEM, and the mechanical properties of leather were also studied. The results show that the prepared polyethylene glycol fatty acid ester sulfosuccinate disodium salt has an emulsion particle size of 4.77 μm, Zeta potential of 97.26 mV, foam volume of 646 mL, critical micelle concentration (cmc) of 8.59×10 -4 mol/L, and contact angle of 63.1°. It is sensitive to Aspergillus niger, Pseudomonas aeruginosa and Staphylococcus aureus, and the minimum inhibitory concentrations (MIC) are 15, 20 and 15 g/L, respectively. The SEM results show that the fiber bundle of the leather is finer and the fiber spacing becomes larger after fat liquoring. The tensile strength of leather is increased from 22.07 MPa to 28.24 MPa, and the elongation at break is decreased from 64.7% to 36.4%.

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    改性油脂乙氧基化物与平平加二元复配体系的性能研究
    Study on performance of modified oil ethoxylates and peregal blend system
    张勇,周婧洁,孙永强,孙晋源,梁慧斌,武华萍
    2019 (3):  162-166.  doi: 10.3969/j.issn.1001-1803.2019.03.005
    摘要 ( 467 )   HTML ( 6 )   PDF(1041KB) ( 744 )  

    通过水溶性、凝固点、润湿、乳化、去污及泡沫性能的测试,研究了非离子表面活性剂改性油脂乙氧基化物(SOE-N-60)与平平加O-20、平平加O-25的二元复配体系的性能。结果表明,25 ℃时,对于总质量分数为70%的SOE-N-60与平平加二元复配产品,SOE-N-60与平平加O-25的质量比大于5:5时;SOE-N-60与平平加O-20的质量比大于4:6时;均能形成均一透明的体系,且产品的凝固点均低于10 ℃;SOE-N-60与平平加O-20及平平加O-25的二元复配体系的去污性能以及对液体石蜡的乳化性能均表现出一定的协同增效作用;复配体系的泡沫略高于单一SOE-N-60。此类复配产品有望用于低温低泡浓缩液体洗涤剂配方中。

    Through the tests of water solubility, freezing point, wetting, emulsification, decontamination and foam properties, the performance of the binary blend system of non-ionic surfactant modified SOE-N-60 with peregal O-25 and peregal O-20 respectively were estimated. The results show that the binary compound system of SOE-N-60 with a total mass fraction of 70% and peregal at 25 ℃ is uniform and transparent and the freezing points of the products are all below 10 ℃, when the mass ratio of SOE-N-60 to peregal O-25 is greater than 5:5 and the mass ratio of SOE-N-60 to peregal O-20 is greater than 4:6. The decontamination performance and liquid paraffin emulsifying performance of the compound products exhibit a certain synergistic effect. The foaming properties of the compound products are slightly higher than the single SOE-N-60. Therefore, the compound products are suitable for the development of low temperature and low foam concentrated liquid detergent.

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    丙烯酸树脂类水性颜料型记号墨水的制备与稳定性研究
    Study on preparation and stability of acrylic resin based waterborne pigment marker ink
    温鲜妮,王立伟,邓维,姜飞,郭亨长
    2019 (3):  167-173.  doi: 10.3969/j.issn.1001-1803.2019.03.006
    摘要 ( 395 )   HTML ( 11 )   PDF(1270KB) ( 583 )  

    通过测试接触角和表面张力优选了表面活性剂和助溶剂,测试墨水附着性优选了附着力促进剂。配制由色浆、丙烯酸树脂、表面活性剂、附着力促进剂等助剂组成的水性墨水,用红外光谱和热重分析对树脂和树脂-附着力促进剂进行表征,测试墨水经高温和低温存放前后的黏度、微观、pH、粒径D50、表面张力等性能变化,最后测试了优选墨水的书写效果。结果表明,表面活性剂OP-10在该墨水体系中降低表面张力的效果最明显,乙醇润湿性最好;附着力促进剂的效果与其分子结构和添加量有关,过量的附着力促进剂易导致墨水稳定性下降,主要体现在微观、黏度、粒径的变化;优选墨水书写效果良好。

    Surfactants and co-solvents were optimized by testing contact angle and surface tension, and adhesion promoters were selected by testing ink adhesion. The aqueous ink composed of additives such as pigment paste, acrylic resin, surfactant, and adhesion promoter. The resin and the resin-adhesion promoter were characterized by Fourier transform infrared spectroscopy (FTIR) and thermogravimetric analysis (TG). The changes of viscosity, microscopic property, pH, particle size of D50, surface tension and other properties of the ink before and after storage at high and low temperatures were tested. Finally, the writing effect of the optimized ink was tested. The results show that the surfactant OP-10 has the most obvious effect on reducing the surface tension in the ink system, and ethanol has the best wettability. The effect of the adhesion promoter is related to its molecular structure and addition amount. However, excessive adhesion promoters could easily lead to the decline of ink stability, which is mainly manifested in the changes of microscopic property, viscosity and particle size. Here we develop a waterborne marker ink which is stable and has excellent adhesion and good writing effect after optimizing the formula.

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    窄分布脂肪醇聚氧乙烯醚的合成研究
    Synthesis of fatty alcohol polyoxyethylene ether with narrow distribution
    田京城,孙永强,郭建国
    2019 (3):  174-177.  doi: 10.3969/j.issn.1001-1803.2019.03.007
    摘要 ( 691 )   HTML ( 3 )   PDF(904KB) ( 471 )  

    在KOH和窄分布专用均相催化剂作用下,分别合成了2种不同平均EO加合度的AEO。根据合成过程中EO的消耗量计算得到理论平均EO加合度,气相色谱法分析了产品组成分布,对常规及窄分布AEO的EO分布、平均EO加合度对分子量分布的影响等进行了研究。结果表明,窄分布AEO气相色谱图中C12(EO)7的峰面积很小,基本看不到C14(EO)7的峰;对于常规及窄分布AEO,AEO2组分中游离脂肪醇质量分数低于AEO1.85,EO加合度为1~4组分的总质量分数则高于AEO1.85;窄分布AEO组分中游离脂肪醇和EO加合度大于4组分的质量分数明显低于常规AEO,而EO加合度为1~4组分的质量分数明显高于常规AEO,分子量分布呈泊松分布,表现出明显的窄分布特点。

    KOH and a homogeneous catalyst were respectively used in the syntheses of fatty alcohol polyoxyethylene ether (AEO) with two degrees of polymerization of ethylene oxide (EO). The theoretical EO degrees was caculated with EO consumption. The product composition was analysed by gas chromatography. The EO distribution of these two kinds of AEO and effects of EO degrees on molecular weight distribution were studied. The results show that in the gas chromatogram of narrow-distribution AEO, the peak area of C12 (EO)7 is very small and the chromatographic peak of C14(EO)7 is barely observable. As to conventional AEO and narrow-distribution AEO, the mass fraction of free fatty alcohol in AEO2 is lower than in AEO1.85, and the total mass fraction of components with EO degrees 1~4 is slightly higher in AEO2 than in AEO1.85. On the other hand, the mass fraction of free fatty alcohol and components with EO degrees above 4 are significantly lower in narrow-distribution AEO than in conventional AEO, while the mass fraction of components with EO degrees 1~4 are much higher in narrow-distribution AEO than in conventional AEO. The components of narrow-distribution AEO show Poisson distribution, indicative of an obvious characteristic of narrow distribution.

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    化妆品美白原料β-熊果苷稳定性研究
    Study on stability of β-arbutin as a cosmetic whitening ingredient
    闫秀芳,张鑫,范倩文
    2019 (3):  178-182.  doi: 10.3969/j.issn.1001-1803.2019.03.008
    摘要 ( 689 )   HTML ( 24 )   PDF(870KB) ( 493 )  

    通过高效液相色谱法检测β-熊果苷降解产物氢醌,考察温度、含量、pH、放置时间以及表皮葡萄球菌、表皮细胞等因素对β-熊果苷稳定性的影响。结果表明,β-熊果苷水溶液在pH=5,温度为40 ℃时相对比较稳定,pH=3时相对不稳定,且随着放置时间的延长,β-熊果苷分解产生的氢醌越多。同时研究发现将表皮葡萄球菌在不同含量的β-熊果苷培养液中培养24 h,β-熊果苷均未分解生成氢醌,说明表皮葡萄球菌不会导致β-熊果苷分解产生氢醌。将表皮细胞放在不同含量的β-熊果苷培养液中培养24 h,有氢醌生成,说明表皮细胞会促进β-熊果苷的分解。进一步研究发现,β-熊果苷原料在不同温度、湿度下均很稳定。在β-熊果苷中加入维生素C、珍珠粉,β-熊果苷的稳定性会下降。

    The β-arbutin degradation product hydroquinone was detected by high performance liquid chromatography to investigate the effects of temperature, content, pH, standing time, Staphylococcus epidermidis and epidermal cells on the stability of β-arbutin. Results show that β-arbutin aqueous solution remains relatively stable under pH of 5 and temperature of 40 ℃, and β-arbutin becomes unstable under pH of 3. The longer the standing time is, the more hydroquinone is produced by the decomposition of β-arbutin. At the same time, it is found that Staphylococcus epidermidis cultured in different content of β-arbutin for 24 h, and β-arbutin does not decompose into hydroquinone, indicating that Staphylococcus epidermidis does not lead to the decomposition of β-arbutin. The epidermal cells were cultured in the medium containing different content of β-arbutin for 24 h, and hydroquinone was generated, indicating that the epidermal cells promote the decomposition of β-arbutin. Further studies show that β-arbutin materials are very stable at different temperatures and humidity. But adding vitamin C and pearl powder into β-arbutin can redu ce the stability of β-arbutin.

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    黄柏盐的制备及其抗氧化抗菌性能研究
    Research on the preparation of “phellodendron beauty salt” and its antioxidative and antibacterial properties
    高天成,孙权,唐娜,杨亚茹
    2019 (3):  183-186.  doi: 10.3969/j.issn.1001-1803.2019.03.009
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    以日晒海盐为载体,配以天然中草药黄柏的有效成分制备了不同配比的黄柏美容盐。对该黄柏盐进行了理化指标、多酚和类黄酮含量、抗氧化性和抗菌性测定。结果表明,黄柏盐中黄柏的质量分数为10%时,该样品盐对DPPH自由基清除率达到50%时的质量浓度(IC50)为124.83 g/L,对酪氨酸酶的IC50为124.83 g/L,对金黄色葡萄球菌和大肠杆菌的IC50分别为131.58和159.69 g/L。本研究为植物盐护肤品的多角度开发与利用提供参考。

    The solar salt and the natural herbal extract from Cortex phellodendri were mixed with various ratios to prepare “phellodendron beauty salt”. Physical and chemical parameters, contents of polyphenols and flavonoids, antioxidative and antibacterial properties of the phellodendron beauty salt were determined. The results show that when the mass fraction of phellodendron bark in the phellodendron beauty salt is 10%, the concentrations of phellodendron beauty salt for 50% inhibition (IC50) against the DPPH free radicals (i.e. scavenging rate of 50%), tyrosinase, Staphylococcus aureus and E. coli are 124.83, 124.83, 131.58 and 159.69 g/L respectively. This study provides a reference to multi-angle development and utilization of plant salt.

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    植物精油的抑菌性探究及其在化妆品中的应用
    Study on antibacterial activity of plant essential oils and its application in cosmetics
    桂雨豪,孟潇,陈庆生,龚盛昭
    2019 (3):  187-192.  doi: 10.3969/j.issn.1001-1803.2019.03.010
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    通过6种精油抑菌性试验,发现肉桂精油、玫瑰精油、甜橙精油具有较好的抑菌性,其中含有高含量醛的肉桂精油抑菌效果最好。研究了在膏霜中添加肉桂精油对防腐体系的影响,实验结果表明:在未添加肉桂精油的膏霜中,防腐剂的用量需添加至0.25%才能对细菌和真菌有较好的抑制效果;在添加了0.01%的肉桂精油的膏霜中,防腐剂的用量只需添加0.1%就能对细菌和真菌有较好的抑制效果。这说明肉桂精油可以降低化妆品中防腐剂的用量。通过皮肤刺激性试验,发现在均能通过防腐测试的前提下,添加了0.01%肉桂精油和0.15%防腐剂的膏霜L/D值为112.26,而只添加了0.25%防腐剂的膏霜L/D值为58.53,说明在化妆品中添加肉桂精油,在降低了防腐剂用量的同时,也降低了化妆品的刺激性。但是,当防腐剂用量均为0.15%时,添加了肉桂精油的膏霜L/D值比未添加肉桂精油的膏霜L/D值略低,这说明肉桂精油本身具有轻微的刺激性。

    Through bacteriostatic tests of six essential oils, it is found that cinnamon essential oil, rose essential oil and sweet orange essential oil have better antibacterial activity, and the cinnamon essential oil which contains high content of aldehyde has the best antibacterial effect. The effect of adding cinnamon oil on the antiseptic system in the cream was studied. The results show that the amount of preservative should be added to 0.25% in the cream without adding cinnamon oil to reach better inhibition effect on bacteria and fungi. In the cream with 0.01% cinnamon essential oil added, the amount of preservative can be adjusted to bacteria and fungi by adding 0.1%. The study demonstrates that the addition of cinnamon essential oil in cosmetics can decrease the dosage of preservatives. Through skin irritation test, it is found that the L/D value of the cream with 0.01% cinnamon essential oil and 0.15% preservative is 112.26, while that of cream with 0.25% preservative is 58.53. This indicates that adding cinnamon essential oil in cosmetics can reduce the amount of preservative and the irritation of cosmetics. However, when the amount of preservatives used is 0.15%, the L/D value of the cream to which the cinnamon essential oil was added is slightly lower than that of the unadded cream, illustrating that the cinnamon essential oil itself is slight irritating.

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    专论与综述
    人参不同部位主要活性成分及其在美容护肤方面的研究进展
    Research progress on the application of main active components from different parts of ginseng in skin care
    熊晨阳,许明良,易帆,孟宏,董银卯
    2019 (3):  193-198.  doi: 10.3969/j.issn.1001-1803.2019.03.011
    摘要 ( 533 )   HTML ( 27 )   PDF(755KB) ( 695 )  

    介绍了人参不同部位的化学成分、主要活性成分、药理作用的差异及其在美容护肤方面的作用。最后对人参作为化妆品原料的发展方向做了展望。

    The chemical composition, main active ingredients, pharmacological effects of different parts of ginseng and their role in beauty and skin care were introduced. Finally, the development direction of ginseng as a raw material for cosmetics was prospected.

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    分析与检测
    化妆品中芦荟苷的测定及其稳定性的研究
    Determination of aloin in cosmetics and its stability
    张强,崔君,顾华,余肖峰,单晓锋,朱鸽
    2019 (3):  199-202.  doi: 10.3969/j.issn.1001-1803.2019.03.012
    摘要 ( 415 )   HTML ( 9 )   PDF(907KB) ( 401 )  

    采用高效液相色谱法,考察了温度、pH、提取溶剂以及共存金属离子等条件对芦荟提取液中芦荟苷稳定性的影响,并通过建立校正曲线测定芦荟化妆品中芦荟苷及其分解产物的含量。样品经5 mL 90%甲醇30 ℃超声提取20 min后,以甲醇-乙腈-0.05%磷酸溶液为流动相梯度洗脱,经C18柱分离,在356 nm波长下随机选取了7种标明添加芦荟成分的化妆品样品进行检测,结果显示,抽检的7种市售芦荟化妆品样品中1件乳液含有芦荟大黄素和大黄酚,1件爽肤水中含有大黄酚,其余均未检出芦荟苷或芦荟苷分解产物。

    The effects of temperature, pH, extraction solvent and metallic ions on the stability of aloin in aloe extract were investigated by HPLC method. The content of aloin and its decomposition products in aloe cosmetics was determined by establishing a calibration curve. The samples were ultrasonically extracted by 5 mL 90% methanol solution at 30 ℃ for 20 minutes, separated on a C18 column by gradient elution using methanol, acetonitrile and 0.05% phosphoric acid as the mobile phases. Then 7 samples of cosmetics labeled aloe components were randomly selected for testing at 356 nm. The results show that one of the seven selected samples of aloe cosmetics contained aloe-emodin and chrysophanol, and one toner contained chrysophanol. And aloin or aloin degradation products were not detected in the rest.

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    HPLC测定儿童化妆品中10种邻苯二甲酸酯类化合物的含量
    Determination of 10 phthalate esters in cosmetics for children by HPLC
    杨永超,闫婧,赵好力宝,李学洋,张园,周磊
    2019 (3):  203-208.  doi: 10.3969/j.issn.1001-1803.2019.03.013
    摘要 ( 385 )   HTML ( 15 )   PDF(939KB) ( 377 )  

    建立了测定儿童化妆品中10种邻苯二甲酸酯类(PAEs)化合物含量的高效液相色谱(HPLC)法。采用Acclaim TM 120-C18(4.6 mm×250 mm, 5 μm)反相柱,流动相为甲醇-乙腈-水,梯度洗脱,流速1.0 mL/min,二极管阵列检测器(DAD),检测波长280 nm。结果表明,在1~100 mg/L范围内,10种PAEs的质量浓度与峰面积呈现良好的线性关系,相关系数均≥0.999 6,10种PAEs的检出限和定量限分别在0.2~5.0 mg/L和0.5~10.0 mg/L范围内。方法验证过程中做了3类化妆品共计8种(化妆水、霜乳类和油状)样品的添加回收,平均回收率为89.2%~106.1%,RSD均小于5%。该方法简便准确,检测限较低,满足实际检测需要,可用于化妆品中PAEs的检测。1个样品有检出,通过3种方法确证为阳性。

    A sensitive and rapid method was developed for the determination of 10 phthalate esters (PAEs) in children’s cosmetics by high performance liquid chromatography (HPLC). The analytes were tested with an Acclaim TM 120-C18 reversed-phase column (4.6 mm×250 mm, 5 μm) under the gradient elution of methanol, acetonitrile and water, and subsequently detected by Diode Array Detector (DAD) at 280 nm. The flow rate was set at 1.0 mL/min. The results show that the ten compounds show good linearity within the concentration range of 1-100 mg/L. The corresponding linear correlation coefficients are all equal to or greater than 0.999 6. And the limits of detection and quantification (LOD and LOQ) located at the range of 0.2-5.0 mg/L and 0.5- 10.0 mg/L, respectively. Recovery experiments were then carried out with 8 cosmetic samples (lotion, cream and oily cosmetics). The average recoveries are between 89.2% and 106.1% with relative standard deviations <5%. Results show that it is a simple and accurate method with low LOD which can serve for cosmetics supervision in determination of the PAEs. One of the eight cosmetics was verified as a positive sample, and three methods were applied to confirm this result.

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