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    2020年, 第50卷, 第1期 刊出日期:2020-01-22 上一期    下一期
    基础研究
    β-环糊精对聚氧乙烯-8-辛基苯基醚紫外光谱抗干扰性能研究
    Study on the anti-interference performance of β-cyclodextrin to the ultraviolet spectrum of Triton X-100
    黄弘毅,尹先清,靖波,王秀军,陈文娟,李赓,石东坡
    2020 (1):  1-7.  doi: 10.3969/j.issn.1001-1803.2020.01.001
    摘要 ( 370 )   HTML ( 52 )   PDF(1355KB) ( 453 )  

    聚氧乙烯-8-辛基苯基醚(曲拉通X-100)和十二烷基三甲基溴化铵(DTAB)之间的相互作用,能对复配水溶液中曲拉通X-100的紫外光谱信号产生明显影响。研究结果表明,DTAB不仅能增强水溶液中曲拉通X-100的吸光度,还能降低曲拉通X-100的表观临界胶束浓度cmc。当DTAB的浓度从0增加到0.100和0.200 mmol/L时,曲拉通X-100的表观cmc从0.187 g/L分别降至0.170和0.154 g/L。在曲拉通X-100和DTAB复配水溶液中,按n(曲拉通X-100) ︰nβ-环糊精)=1︰1加入β-环糊精,不仅能有效减少曲拉通X-100和DTAB间的相互作用而且可以增强曲拉通X-100紫外光谱信号强度,二者复配水溶液中曲拉通X-100回收率从92.0%~97.3%增加到98.8%~102.2%,曲拉通X-100浓度的检测精度显著提高。Job’s实验结果和FT-IR结果表明,曲拉通X-100分子进入β-环糊精分子空腔形成包结物,是β-环糊精消除各种相互作用对曲拉通X-100紫外光谱产生干扰的主要原因。

    The interactions between polyethylene glycol tert-octylphenyl ether (Triton X-100) and dodecyl trimethyl ammonium bromide (DTAB) has significant effects on the ultraviolet spectral signals of Triton X-100 in the aqueous mixture. The results show that DTAB can increase the absorbance of Triton X-100 in aqueous solution and also has a remarkable influence on the apparent critical micelle concentration (cmc) of Triton X-100, where the apparent cmc values of Triton X-100 are reduced from 0.187 g/L to 0.170 and 0.154 g/L when the concentration of DTAB increase from 0 to 0.100 and 0.200 mmol/L, respectively. Adding β-cyclodextrin (β-CD) by molar ratio of 1∶1 between Triton X-100 and β-CD in the aqueous mixture of Triton X-100 and DTAB can not only effectively reduce the interactions between Triton X-100 and DTAB, but also enhance the ultraviolet signal intensity of Triton X-100. Thus, the recovery rates of Triton X-100 change from 92.0%-97.3% to 98.8%-102.2%, which indicate that the measurement accuracy of Triton X-100 has been greatly improved. The results of Job’s experiment and infrared spectrum show that, β-CD can eliminate the interference (arising from other coexisting components) to the UV spectra of Triton X-100, which is primarily attributed to the formation of inclusion complexes with Triton X-100 molecules entering into the cavities of β-CD molecules.

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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(Ⅰ)—功能性两亲聚合物分子结构设计
    Study on the design and synthesis of amphiphilic polymers and their synergistic systems (Ⅰ) Molecular structure design of functional amphiphilic polymers
    康万利,王芳,杨红斌,张向峰,李梦栏
    2020 (1):  8-13.  doi: 10.3969/j.issn.1001-1803.2020.01.002
    摘要 ( 319 )   HTML ( 6 )   PDF(786KB) ( 315 )  

    综述了近些年功能性两亲聚合物驱油剂的研究进展。主要概述了两亲聚合物在分子结构设计方面取得的研究成果,包括疏水单体设计和功能单体设计两方面的内容,疏水单体的设计阐述了孪尾型、苯环型和双取代型3种,功能单体的设计阐述了表面活性单体、甜菜碱单体和耐温抗盐单体3种。

    The research progress on the functional amphiphilic polymers as oil-displacing agents in recent years is summarized, including the research results in molecular structure design of amphiphilic polymers. The research progress mainly involves the design of hydrophobic monomers and functional monomers. Design of hydrophobic monomers consists of double-tailed monomers, benzene ring monomers and double substitution monomers. Design of functional monomers consists of surface active monomers, betaine monomers and temperature- and salt-resistant monomers.

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    化妆品功效评价(Ⅻ)—皮肤生理学检测在化妆品功效评价中的应用
    Efficacy evaluation of cosmetics (Ⅻ)Application of cutaneous biological test in efficacy evaluation of cosmetics
    马雪,宋艳青,盘瑶,赵华,卢永波,范展华
    2020 (1):  14-19.  doi: 10.3969/j.issn.1001-1803.2020.01.003
    摘要 ( 812 )   HTML ( 39 )   PDF(864KB) ( 1868 )  

    阐述了皮肤生理学检测的概念,介绍了皮肤形态组、脂质组、微生物组、功能组等生理学检测方法和指标在化妆品功效评价中的应用,为化妆品进行人体功效评价时皮肤生理学指标的选择提供了参考和指导,并对皮肤生理学检测技术的现状和发展趋势进行了总结和展望。

    The concept of cutaneous biological test was summarized, and the application of cutaneous biological test methods and indicators in the efficacy evaluation of cosmetics including morphology, lipidomics, microbiome, and physiological function were introduced. It provided a reference and guidance for the selection of appropriate cutaneous biological indicators in the evaluation of efficacy of various cosmetics. The current status and development trends of cutaneous biological test were summarized and prospected.

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    开发与应用
    烷基糖苷磺基琥珀酸酯盐与烷基糖苷的复配性能和相行为
    Performance and phase behavior of the mixture of alkyl polyglycoside sulfosuccinate and alkyl polyglycoside
    周媛,杨秀全,张军
    2020 (1):  20-25.  doi: 10.3969/j.issn.1001-1803.2020.01.004
    摘要 ( 398 )   HTML ( 8 )   PDF(1311KB) ( 359 )  

    分别对烷基糖苷磺基琥珀酸酯盐(APG-SS)和烷基糖苷(APG)不同摩尔比复配体系的表面张力和泡沫性能进行研究,同时研究烷基糖苷/烷基糖苷磺基琥珀酸酯盐/水三元体系的相行为。结果表明:APG-SS与APG摩尔比为2∶8时,表面张力达到27.90 mN/m,cmc=0.044 mmol/L,Γmax=10.86 μmol/m 2,Amin=0.15 nm 2,与其他摩尔比复配体系相比,表面性能较好,具有较好的协同效应。在蒸馏水和硬水中,APG-SS与APG摩尔比为2∶8和4∶6的复配体系的起泡性能均优于单一表面活性剂,具有较好的协同效应。同时,复配体系的泡沫稳定性优于APG,可改善APG的抗硬水能力。APG-SS/APG/H2O体系的三元相图出现胶束相、胶束-液晶共存区和双水相区。

    The mixtures of alkyl polyglycoside (APG) and alkyl polyglycoside sulfosuccinate (APG-SS) with different mixing ratios were studied by measuring their surface activity and foaming properties. The phase behavior of the ternary system of APG/APG-SS/H2O was also studied. The results show that the best synergism is found in surface activity (γcmc=27.90 mN/m, cmc=0.044 mmol/L, Γmax=10.86 μmol/m 2, Amin=0.15 nm 2) when nAPG-SSnAPG=2∶8. The mixed system has higher foaming ability in distilled water and hard water than single surfactant when nAPG-SSnAPG=2∶8 and 4∶6, so it has synergism. At the same time, the foam stability of the mixed system is better than APG, which can improve the hard water resistance of APG. The phase diagrams of the APG-SS/APG/H2O ternary systems were characterized by micellar phase, a region where lamellar liquid crystal and micellar phases coexisted and a region of “aqueous two-phase”.

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    SiO2 纳米颗粒对水相泡沫稳定性的影响
    Effects of SiO2 nanoparticles on the stability of aqueous foams
    张阳,燕永利,奚琪,于长龙,寇卫伟
    2020 (1):  26-31.  doi: 10.3969/j.issn.1001-1803.2020.01.005
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    采用SiO2纳米颗粒分别与阴离子表面活性剂十二烷基硫酸钠(SDS)、阳离子表面活性剂十六烷基三甲基溴化铵(CTAB)、非离子表面活性剂十二烷基醇聚氧乙烯(3)醚(AEO-3)复配制备水相泡沫,研究了发泡体积、半衰期和微观结构的变化规律,以揭示SiO2纳米颗粒对水相泡沫稳定性的影响机理。结果表明,在表面活性剂质量分数一定的条件下,随着纳米颗粒质量分数的增加,泡沫稳定性逐渐增强,当纳米颗粒质量分数为0.3%时,发泡体积达最大值,含气率分别为78.9%,78.4%和78.8%。与单组分质量分数分别为0.3%,0.3%和15%的SDS、CTAB、AEO-3体系相比,发泡体积未受影响,半衰期分别为9.0,8.2和360 min,提高了20%,28.1%和71.4%,泡沫的稳定性得到了不同程度的改善。

    SiO2 nanoparticles was mixed with anionic surfactant sodium dodecyl sulfate (SDS), cationic surfactant cetyltrimethylammonium bromide (CTAB) and nonionic surfactant dodecyl alcohol polyoxyethylene (3) ether (AEO-3), respectively, to prepare the aqueous foams thereof. The variations of foaming volume, half-life and microstructure were determined to reveal the influence of SiO2 nanoparticles on the stability of aqueous foams. The results showed that when the mass fraction of the surfactant is constant, the foam stability gradually increase with the increase of the mass fraction of nanoparticles. When the mass fractions of the nanoparticles are 0.3%, the foaming volumes reached maxima with gas contents of 78.9%, 78.4% and 78.8%, respectively. Compared with the single systems of SDS, CTAB and AEO-3 at surfactant concentrations of 0.3%, 0.3% and 15%, respectively, these experimentally prepared foams did not affect the foaming volumes but the foam stability had been variously improved (the half-lives are 9.0 min, 8.2 min and 360 min, which are increase by 20%, 28.1% and 71.4%, respectively).

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    梨果仙人掌籽油化学成分及其抗氧化活性和刺激性的研究
    Studies on chemical constituents, antioxidant and irritancy of Opuntia ficus-indica L. seed oil
    邹小灵,刘环宇
    2020 (1):  32-37.  doi: 10.3969/j.issn.1001-1803.2020.01.006
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    以梨果仙人掌籽油为研究对象,通过气-质联用技术(GC-MS)分析其化学成分;以1,1-二苯基-2-三硝基苯肼(DPPH)、羟自由基、超氧阴离子、总还原力、总抗氧化能力为指标评价其体外抗氧化活性;通过鸡胚绒毛尿囊膜试验和人体重复性开放型涂抹试验评价其刺激性。结果表明,从梨果仙人掌籽油中鉴定出16种质量分数大于0.1%的化合物,占总质量的94.02%。其中质量分数大于1%的有亚油酸(C18∶2) 60.42%、十六酸(C16∶0) 15.20%、硬脂酸(C18∶0) 5.57%、γ-谷甾醇4.34%、亚麻酸(C18∶2) 1.89%、油酸(C18∶1) 1.48%、顺-7-十六碳烯酸(C16∶1) 1.13%。梨果仙人掌籽油具有良好的抗氧化能力,对DPPH自由基、羟自由基、超氧阴离子、总还原力和总抗氧化能力各指标的半数清除率IC50分别为5.11,0.79,3.19,1.12和1.49 g/L。鸡胚绒毛尿囊膜试验和人体重复性开放型涂抹试验显示梨果仙人掌籽油无刺激性。

    Taking Opuntia ficus-indica L . seed oil as the research object, its chemical constituents was analyzed by gas chromatography-mass spectrometry (GC-MS). The antioxidant activities in vitro of the Opuntia ficus-indica L. seed oil were evaluated by 1,1-diphenyl-2-picrylhydrazyl (DPPH), hydroxyl radical, superoxide radical, total reductive capacity and total antioxidant capacity as indicators. Its irritancy was evaluated by hen’s egg test on the chorioallantoic membrane and repeated open application test. The results show that 16 compounds with a mass fraction greater than 0.1% are identified from the Opuntia ficus-indica L. seed oil accounting for 94.02% of the total mass. Among them, the mass fraction more than 1%: linoleic acid (C18∶2) 60.42%, hexadecanoic acid (C16∶0) 15.20%, stearic acid (C18∶0) 5.57%, γ-sitosterol 4.34%, linolenic acid (C18∶2) 1.89%, oleic acid (C18∶1) 1.48%, and cis-7-hexadecenoic acid (C16∶1) 1.13%. The Opuntia ficus-indica L . seed oil has strong antioxidant activity capacity, the half clearance rate (IC50) of DPPH free radical, hydroxyl free radical, superoxide anion, total reducing power and total antioxidant capacity are 5.11, 0.79, 3.19, 1.12 and 1.49 g/L, respectively. The hen’s egg test on the chorioallantoic membrane and repeated open application test show that Opuntia ficus-indica L. seed oil is non-irritating.

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    阿胶开发为化妆品原料的有效成分及安全性分析
    The active ingredients and safety analysis of colla corii asini as a cosmetic raw material
    帖航,廖峰,王超,闫妍,解晓,苏宁
    2020 (1):  38-43.  doi: 10.3969/j.issn.1001-1803.2020.01.007
    摘要 ( 484 )   HTML ( 11 )   PDF(1121KB) ( 467 )  

    以东阿阿胶作为研究对象,采用高分辨质谱技术对其主要功效成分进行鉴定,同时对其进行较为系统的化妆品安全性评估研究。结果显示,阿胶中含有较为丰富的氨基酸、维生素、糖类和脂质等功效营养活性成分,具有良好的开发价值。当阿胶溶液的料液比在1∶100 (g∶mL)以下时,其对表皮及真皮细胞均无明显细胞毒性作用,无光毒性作用,无眼刺激性/腐蚀性作用,无皮肤刺激性/腐蚀性作用。结果表明东阿阿胶具有开发为化妆品原料的功效价值且具有作为化妆品原料所必须具备的基础安全性。

    Ejiao (Dong’e Ejiao) was analyzed by high resolution mass spectrum (HRMS) to identify its components, and its safety as a cosmetic raw material was systematically evaluated. The results showed that Ejiao contained abundant functional and nutritive ingredients such as amino acids, vitamins, sugars and lipids, which had good development value. No obvious cytotoxic effect on epidermis and dermal cells was observed when the solid to liquid ratio of Ejiao solution was below 1∶100 (g∶mL); there was no phototoxic effect, eye irritation/corrosive effect, or skin irritation/corrosive effect. The results showed that Ejiao had the efficacy value of being a cosmetic raw material with sufficient basic toxicological safety.

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    基于大数据聚类的化妆品包装符号元素特征提取
    Feature extraction of cosmetic packaging symbol elements based on big data clustering
    吴芳菲
    2020 (1):  44-48.  doi: 10.3969/j.issn.1001-1803.2020.01.008
    摘要 ( 340 )   HTML ( 5 )   PDF(1133KB) ( 418 )  

    研究了基于大数据聚类的化妆品包装符号元素特征提取方法。初始化处理水平集函数,获取化妆品包装符号元素图像的局部标准差图像,根据余弦相似性确定局部标准差图像像素点在轮廓曲线上的演化方向,水平集演化改进SPF函数,完成符号元素分割;计算大数据的离散样本频谱特征,由置信度获取数据聚类中心的粒子最优解的向量矩阵,完成数据聚类;结合卷积神经网络和AutoEncoder,通过卷积、过滤以及池化操作,在输出层存在的节点中获取最大激活值,实现化妆品包装符号元素特征的提取。实验结果表明,所提方法的特征提取时间较短、特征辨识力有所提高且提取准确率较高。

    The feature extraction method of cosmetic packaging symbol elements based on big data clustering was proposed. The level set function was initialized to obtain the local standard deviation image of cosmetic packaging symbol element image. The evolution direction of local standard deviation image pixels on contour curve was determined according to the cosine similarity. The level set evolution improved the SPF function to complete the symbol element segmentation. The discrete sample spectrum characteristics of big data were calculated, and the vector matrix of the particle optimal solution of the data clustering center was obtained by the confidence degree to complete the data clustering. By combining convolution neural network and AutoEncoder, the maximum activation value was obtained in the nodes existing in the output layer through convolution, filtering and pooling operations, and the feature extraction of cosmetic packaging symbol elements was realized. The experimental results show that the proposed method has shorter feature extraction time, higher feature recognition ability and higher extraction accuracy.

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    专论与综述
    我们该如何看待全氟或多氟烷基物质(PFAS)?
    Do we need to regard PFAS as evil? Our points of view
    邢航,窦增培,肖子冰,肖进新
    2020 (1):  49-53.  doi: 10.3969/j.issn.1001-1803.2020.01.009
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    全氟辛基磺酰氟/全氟辛烷磺酸/全氟辛烷磺酸盐及其衍生物(PFOS)和全氟辛酸/全氟辛酸盐及其衍生物(PFOA)在全球及生物圈内的广泛分布引起了环境学家和毒理学家的批判,国际社会已出台相应法案和行动措施对其进行淘汰和限制,而如今国际上一些学者又将目标扩大到了整个全氟或多氟烷基物质(PFAS)领域,公众也对此产生了激烈的争论。并非所有PFAS都有明确的健康风险,但它们的通性是非常稳定,难于降解,因而受人诟病。近日在全球化学化工领域最具影响力的新闻杂志“化学与工程新闻”(Chemical & Engineering News, C&EN)的网站上,发表了题目为《如何摆脱PFAS》的文章。其中的很多观点反映了主流看法,即反对“一刀切”,应对具体物质根据其必要性和可替代性进行区分对待,同时反对无限制的生产和应用PFAS,积极寻求替代品。我们赞同该文的思路,但也有异议,主要体现在视角的差异以及区分标准上,以及对其中激进观点的反对。《如何摆脱PFAS》一文更多侧重来自环境学家的主张,我们则是PFAS的科研工作者及技术开发者,同时也是PFAS一个小量的、细分产品的生产者;上文的作者采取的是发达国家视角,我们则认为发展中国家要更细致地、深入地看待分类的问题。中国应努力在这场标准制定的历史进程中积极参与,结合自身实际状况,不要盲从,制定出适合自己的执行方案,尤其不能冒进。

    The ubiquitous distribution of PFOS and PFOA in the globe and biota has induced the criticism from environmental scientists and toxicologists. The international community has established laws and supervision measures to eliminate PFOS and PFOA. Now some scholars begin to fire at the whole class of PFAS (per-,polyfluoroalkyl substances) , and the public argues intensely (fear arise from being not understood). Not all PFAS are verified with health risk, but they are surely blamed by being too stable and thus too difficult to degrade. Recently, a paper titled “How to say goodbye to PFAS” is published on the website of the world’s most influential news magazine in the field of chemical industry named Chemical & Engineering News (C&EN). Many of the view points therein reflect the prevailing opinion, which is against “one-size-fits-all”, that specific substances should be treated differently according to their necessity and substitutability, and that the unchecked growth in production and application of PFAS should be turned around, and that substitutes should be actively pursued. We agree with the thought of this paper, but also have objections mainly addressed on the different view angle and the standard of classification. The author of that paper has focused on the views of environmentalists, while we are researchers and technology developers of PFAS, as well as a manufacturer of some narrow-category PFAS products; the author of that paper takes the perspective of developed countries, while we consider that developing countries should weigh well the way of categorization more carefully and deeply before action. China should positively participate in this historical argument of standard-setting, take into account our own actual conditions, and work out a suitable implementation plan, particularly, do not blindly follow or go ahead radically and rashly.

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    分析与检测
    氧化型染黑用途染发剂中32种染料监测结果分析
    Analysis on the determination results of 32 kinds of dyes used in oxidized blackening hair dyes
    李彬,张伟清,刘慧锦,侯俐南,乔亚森,王海燕
    2020 (1):  54-58.  doi: 10.3969/j.issn.1001-1803.2020.01.010
    摘要 ( 592 )   HTML ( 10 )   PDF(804KB) ( 487 )  

    采用《化妆品安全技术规范》(2015年版)中对苯二胺等32种组分的测定方法对市售25批氧化型染黑用途染发剂进行检测,并对组分检测结果、批件配方、标签标示三者进行比对,研究分析该类染发剂的生产和质量状况,发现风险点并提出合理的监管建议。结果表明,32种组分中涉及的8种禁用组分均未检出,24种准用染发剂组分中的苯基甲基吡唑啉酮有6批样品超限量添加,17批样品“检测结果与批件配方”不一致,16批样品“检测结果与标签标示”不一致,5批样品“批件配方与标签标示不一致;总体问题样品17批,问题发现率为68%。针对结果提出加强对含苯基甲基吡唑啉酮组分染发剂的监督抽检,开展包装、标签标示专项整顿的监管建议,并对超限量添加苯基甲基吡唑啉酮的原因进行分析。

    The 25 batches of commercially available oxidized blackening hair dyes were collected, and the contents of 32 selected chemical substances including p-Phenylenediamine in these products were assessed according to Safety and Technical Standards for Cosmetics (2015 edition). The content analysis results were compared with the approved formulas and labels of each product. The purpose of the survey was to gather information about the production and quality of this kind of hair dyes on domestic market, with the goal of uncovering the safety risks and providing supervision suggestions. The result shows that none of the eight prohibited components involved in the 32 components are detected in all investigated products. With regard to the 24 permitted hair dye components, phenyl methyl pyrazolone was found to exceed the permitted limit in 6 batches of the products. 17 batches of samples were inconsistent with the test results and the approved formulas, 16 batches of samples were inconsistent with the test results and the labels, and 5 batches of samples were inconsistent with the approved formulas and the labels. 17 batches of samples in total were problematic, with the problem discovery rate of 68%. According to the results, it is necessary to strengthen the inspection of hair dyes containing phenyl methyl pyrazolone, and carry out the special rectification in packages and labels. The reasons for the excessive addition of phenyl methyl pyrazolone was analyzed in the survey.

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    高效液相色谱法测定口腔护理产品中卡松含量及质谱确证
    Determination of kathon content in oral care products by high performance liquid chromatography and verification by HPLC-MS/MS
    王聪,闫妍,王超,王秀娟,苏宁,余梦圆
    2020 (1):  59-63.  doi: 10.3969/j.issn.1001-1803.2020.01.011
    摘要 ( 429 )   HTML ( 2 )   PDF(1058KB) ( 386 )  

    建立了口腔护理产品中卡松含量的高效液相色谱分析方法。以水和甲醇溶解,超声提取过滤后,选用C18 (250 mm×4.6 mm,5 μm)色谱柱,流动相为甲醇和水(45∶55,V/V),以275 nm波长在15 min内进行定量分析。甲基异噻唑啉酮(MIT)和甲基氯异噻唑啉酮(CMIT)分离效果良好,其中甲基异噻唑啉酮的线性范围为0.07~10 mg/L(R 2>0.999 0),检出限和定量限分别为0.2和0.7 mg/kg,实际样品中加标回收率和相对标准偏差范围分别为96.1%~101.4%和1.1%~5.6%;甲基氯异噻唑啉酮的线性范围为0.2~30 mg/L(R 2>0.999 0),检出限和定量限分别为0.6和2 mg/kg,实际样品中加标回收率和相对标准偏差范围分别为96.0%~101.8%和1.0%~2.9%。阳性样品可用液相色谱-串联四级杆质谱(HPLC-MS/MS)进行确证。该分析方法简便、准确、快速,适用于口腔护理产品中卡松含量的测定。

    A high performance liquid chromatography method for the determination of kathon in oral care products was established. It was dissolved in water and methanol, and after ultrasonic extraction and filtration, a column of C18 column (250 mm×4.6 mm, 5 μm) was used. The mobile phase was methanol and water (45∶55,V/V) and the quantitatively analysis was carried out at a wavelength of 275 nm in 15 minutes. The results show that methylchloroisothiazolone (CMIT) and methylisothiazolone (MIT) have good separation performance, among which the linear range is 0.07-10 mg/L (R 2>0.999 0). The limits of quantitation (LOQs) and detection (LODs) are 0.7 and 0.2 mg/kg, respectively. The recovery rate of the actual sample is 96.1%-101.4%, and the relative standard deviation (RSDs) is between 1.1% and 5.6%. The linear range of methylchloroisothiazolone is 0.2-30 mg/L (R 2>0.999 0). The limits of quantitation (LOQs) and detection (LODs) are 2 and 0.6 mg/kg, respectively. The spiked recovery and relative standard deviation range of the actual samples are 96.0%-101.8% and 1.0%-2.9%, respectively. The detection of the kathon sample can be confirmed by liquid chromatography-tandem quadrupole mass spectrometry (HPLC-MS/MS). The analytical method is simple, accurate and rapid, and it is suitable for the determination of kathon in oral care products.

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    UPLC-MS/MS测定化妆品中15种禁用物质
    Determination of fifteen prohibited substances in cosmetics by ultra performance liquid chromatography-triple quadrupole mass spectrometry
    曹海荣,李晓宇,薛晓康
    2020 (1):  64-70.  doi: 10.3969/j.issn.1001-1803.2020.01.012
    摘要 ( 343 )   HTML ( 6 )   PDF(885KB) ( 300 )  

    建立了同时测定化妆品中苯海拉明、曲吡那敏和氯苯那敏等15种禁用物质的超高效液相色谱-串联质谱(UPLC-MS/MS)分析方法。采用Waters Acquity UPLC ?BEH C18色谱柱(1.7 μm×2.1 mm×50 mm)进行分离,以甲醇和乙酸铵-甲酸水溶液为流动相梯度洗脱,流速为0.4 mL/min,进样量为3 μL,在电喷雾正离子模式下(ESI +),采用多反应监测(MRM)模式进行定性和定量。结果表明,所建立的方法在相应的浓度范围内线性关系良好,线性相关系数为0.999 3~0.999 9,加标回收率在87.21%~99.39%(n=3)之间,相对标准偏差为2.28%~5.27%(n=6),检出限为0.004 3~0.239 2 mg/kg,定量限为0.014 3~0.797 2 mg/kg。本方法准确、可靠,适用于化妆品中多种禁用物质的同时测定。

    An analytical method of ultra performance liquid chromatography-triple quadrupole mass spectrometry (UPLC-MS/MS) was developed for the simultaneous determination of 15 prohibited substances (diphenhydramine, tripelennamine, chlorpheniramine, etc.) in cosmetics. The UPLC separation was carried out on a Waters Acquity UPLC? BEH C18 column (1.7 μm × 2.1 mm × 50 mm) by gradient elution using methanol and ammonium acetate-formic acid solution. The flow rate was 0.4 mL/min and the sample injection amount was 3 μL. The electrospray ionization source in positive ion mode (ESI +) was used for qualitative analysis and quantitative analysis of fifteen prohibited drugs in the multiple reaction monitoring (MRM) mode. The established method exhibited a good linear relationship in the corresponding concentration range. The linear correlation coefficient is 0.999 3-0.999 9; the recoveries of standard addition are between 87.21%-99.39% (n=3); the relative standard deviation is 2.28%-5.27% (n=6); the detection limit range is 0.014 3-0.239 2 mg/kg; the limit of quantification range is 0.004 3-0.797 2 mg/kg. The method is accurate and reliable, and is suitable for simultaneous determination of various prohibited substances in cosmetics.

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