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2020年, 第50卷, 第11期　刊出日期：2020-11-22 上一期    下一期

基础研究

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乳化剂及油脂结构对O/W/O多重乳液形成及稳定的影响 Effects of the structure of emulsifiers and oils on the formation and stability of O/W/O multiple emulsions 张倩洁,段国兰,张婉萍 2020 (11):  735-742.  doi: 10.3969/j.issn.1001-1803.2020.11.001 摘要 ( 614 )   HTML ( 44 )   PDF(3322KB) ( 626 )   利用两步法制备O/W/O多重结构乳状液,通过选择3种亲油性乳化剂、3种亲水性乳化剂和直链烷烃、支链烷烃、酯类3种不同类别的6种油脂,系统分析乳化剂及油脂结构对W/O界面和O/W界面的影响,进而分析其对O/W/O多重乳液形成及稳定的影响。研究结果表明:对于W/O界面而言,W/O乳化剂结构对O/W/O多重结构的形成起着至关重要的作用,非极性的直链或支链油脂制备得到的多重结构稳定性更佳,且油脂极性越低体系的稳定性越好。与W/O乳化剂不同,O/W乳化剂在各类油脂中均可以形成O/W/O多重结构,但体系的稳定性受到了油脂黏度、极性以及与乳化剂相溶性等多方面因素影响,油脂黏度越高、极性越小,越有利于体系的长久稳定。 O/W/O multi-structure emulsions were prepared by two-step method. By selecting three lipophilic emulsifiers, three hydrophilic emulsifiers, and six different types of oils （linear alkanes, branched alkanes, and esters grease）, the effects of the structure of emulsifiers and oils on the W/O and O/W interfaces were systematically analyzed, as well as their effects on the formation and stability of O/W/O multiple emulsions. The results showed that, for the W/O interface, the structure of W/O emulsifier played a crucial role on the formation of multiple structures of O/W/O. The multiple structures prepared with non-polar linear or branched oils had better stability, and the lower the polarity of the oil, the better the stability of the system. For the O/W interface, all of the three O/W emulsifiers could form O/W/O multiple structures in various oils, but the stability of the system was affected by various factors such as the viscosity and polarity of oils and the solubility of emulsifiers. Higher viscosity and smaller polarity of the oils would facilitate the long-term stability of the system. 数据和表 | 参考文献 | 相关文章 | 计量指标

科技讲座

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两亲聚合物设计合成及其增效体系研究（XI）——两亲聚合物凝胶 Study on the design and synthesis of amphiphilic polymers and their synergistic systems (XI) Amphiphilic-polymer gels 杨红斌,康万利,李哲,Bauyrzhan Sarsenbekuly,蒋海壮,王嘉林 2020 (11):  743-748.  doi: 10.3969/j.issn.1001-1803.2020.11.002 摘要 ( 264 )   HTML ( 7 )   PDF(1288KB) ( 374 )   在对两亲聚合物凝胶优势特点介绍的基础上,探讨了聚合物凝胶体系各构筑组分以及应用油藏环境等对两亲聚合物凝胶成胶性能的影响机制及影响规律。最后提出了两种两亲聚合物复合凝胶体系的构筑方法:无机颗粒增强型两亲聚合物复合凝胶和主客体包合型两亲聚合物复合凝胶,最后对两亲聚合物凝胶的发展趋势进行了展望,本文可为两亲聚合物凝胶的设计及应用提供理论和技术基础。 Based on the introduction of characteristics and advantages of amphiphilic-polymer gels, the influencing mechanism and influencing rules of the components of polymer gel system and the reservoir application environment on the gel performance of amphiphilic-polymer gels have been discussed. Two methods for constructing composite gels based on amphiphilic polymers have been studied, including the methods of “inorganic-particle-reinforced” type and of “host-guest inclusion” type. Then the development trend of amphiphilic-polymer gels has been prospected. This work can provide a theoretical and technical basis for the design and application of amphiphilic-polymer gels. 数据和表 | 参考文献 | 相关文章 | 计量指标

开发与应用

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烷基化壳聚糖硫酸盐的制备及性能研究 Preparation and properties of alkylated chitosan sulfate 贾振勇,李萍,杨效益,郭朝华,李建波 2020 (11):  749-755.  doi: 10.3969/j.issn.1001-1803.2020.11.003 摘要 ( 251 )   HTML ( 7 )   PDF(1487KB) ( 452 )   通过希夫碱反应并还原、硫酸化和中和反应,合成了两种壳聚糖表面活性剂:十二烷基壳聚糖硫酸盐（D12CTS）和十烷基壳聚糖硫酸盐（D10CTS）。通过红外光谱（FT-IR）、核磁共振氢谱（1H NMR）、元素分析（EA）和热重分析（TGA）鉴定了它们的结构。结果表明,D10CTS和D12CTS的烷基化度分别为0.77和0.52,硫酸化度分别为1.35和1.79。通过表面张力和接触角测量表明D10CTS和D12CTS具有良好的表面活性和铺展性,临界胶束浓度（cmc）分别为0.69和0.49 g/L,最低表面张力（γcmc）分别为39.50和35.75 mN/m。目标产物具有一定的起泡性能和乳化能力,该表面活性剂为低泡型表面活性剂,有望在化妆品领域发挥潜在的应用。 Two kinds of chitosan surfactants, dodecyl chitosan sulfate （D10CTS） and decyl chitosan sulfate （D12CTS） were synthesized by Schiff base reaction, reduction, sulfation and neutralization reaction. Their structures were identified by infrared spectroscopy （FT-IR）, H NMR spectroscopy（1H NMR）, elemental analysis （EA）, and thermogravimetric analysis （TGA）. The results show that the degrees of alkylation are 0.77 and 0.52, and the degrees of sulfation are 1.35 and 1.79, respectively. Favourable surface activity and spreadability of D10CTS and D12CTS were evidenced by surface tension and contact angle measurements. The critical micelle concentrations （cmc） are 0.69 and 0.49 g/L, and the minimum surface tension γcmc are 39.50 and 35.75 mN/m, respectively. The target products possess certain foaming properties and emulsification performance. The surfactants are low-foaming and are expected to play a potential application in the field of cosmetics. 数据和表 | 参考文献 | 相关文章 | 计量指标

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苏里格气田典型区块凝析油采出液用破乳剂的筛选及评价 Screening and evaluation of demulsifiers for condensate fluids in typical blocks of Sulige Gas Field 王田田,李明星,于淑珍,张振云,马建中,吕斌 2020 (11):  756-761.  doi: 10.3969/j.issn.1001-1803.2020.11.004 摘要 ( 294 )   HTML ( 6 )   PDF(1379KB) ( 274 )   通过对苏里格气田乌*站采出液用破乳剂的筛选评价,系统研究了10种典型破乳剂在破乳温度为25 ℃,破乳剂投加量为1 500 mg/L下对乌*站采出液的破乳效果。结果表明:SW-70与ZX-F302破乳剂的脱水效果最佳,脱水率分别为91.00%和88.30%;VT-1与ZX-F302破乳剂的脱油效果最佳,脱油率均为75.80%。进一步将上述优选出的脱水型破乳剂与脱油型破乳剂进行复配,当SW-70和VT-1的质量比为1:1时,获得破乳效果最佳的复配破乳剂配方,且破乳5 h的脱水率达96.20%,脱油率为90.25%,脱出水中含油率为16.98 mg/L,采出液中的凝析油-水-固体机械杂质悬浮物实现三相分离,油/水界面整齐,固体机械杂质悬浮物絮沉在底部,达到油净水清的效果。 Through screening and evaluating the demulsifiers used for the produced fluids of Wu * Station in Sulige Gas Field, 10 typical demulsifiers were systematically studied at the demulsification temperature of 25 ℃ and the demulsifier dosage of 1 500 mg/L. The results showed that SW-70 and ZX-F302 demulsifiers had the best dehydration effect, with dehydration rates of 91.00% and 88.30%, respectively; VT-1 and ZX-F302 demulsifiers had the best deoiling effect, both with a deoiling rate of 75.80%. The above-selected demulsifiers were further compounded to prepare high-efficiency demulsifiers. When the mass ratio of SW-70 to VT-1 was 1:1, a compound demulsifier with the best demulsification effect was obtained. After 5 hours of demulsification, the dehydration rate was 96.20%, and the deoiling rate was 90.25%, and the oil content in the water phase was 16.98 mg/L. The condensate, water and solid-particle impurities in the condensate produced fluid were separated into three phases. The condensate-water interface was neat, and the solid-particle impurities were flocculated at the bottom. After demulsification, the condensate and water were purified. 数据和表 | 参考文献 | 相关文章 | 计量指标

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三甲基硅基普鲁兰多糖的制备与性能 Preparation and properties of trimethylsilyl pullulan 姬迎迎,杨成 2020 (11):  762-770.  doi: 10.3969/j.issn.1001-1803.2020.11.005 摘要 ( 305 )   HTML ( 11 )   PDF(1619KB) ( 573 )   以N,O-双（三甲基甲硅烷基）乙酰胺（BSA）作为甲硅烷基化试剂,合成了三甲基硅基普鲁兰多糖,并用红外、核磁及XPS表征。当n（P-OH）:n（BSA）=9:15时,取代度高达2.89。三甲基硅基普鲁兰多糖具有优异的成膜性,膜的拉伸强度及断裂伸长率随取代度增加而降低,但当取代度超过1.55时,不再随取代度增加而下降。随取代度的增加,膜与水及皮脂的接触角随之增大,疏水的同时有一定的抗皮脂性。三甲基硅基普鲁兰多糖能乳化水相形成油包水乳液,研究了取代度和油相种类对乳化性能的影响,表明取代度为1.91,乳化性能最佳。对比乳化剂EM90形成的乳液,虽然三甲基硅基普鲁兰多糖形成乳液的粒径较大,但乳液黏度高,稳定性更好。 Trimethylsilyl pullulan was synthesized using N, O-bis（trimethylsilyl）acetamide （BSA） as the silylation agent. The structure of the modified pullulan was characterized by 1H NMR, FT-IR and XPS. When n（P-OH）:n（BSA） was 9:15, the degree of substitution（DS） was as high as 2.89. Trimethylsilyl pullulan has excellent film-forming properties. The tensile strength and elongation at break of the film decrease with the increase of DS, but this phenomenon disappears when the DS is above 1.55. As the DS increases, the contact angle of the membrane with water and sebum increases, and the hydrophobic film has a certain degree of sebum resistance. Trimethylsilyl pullulan can emulsify the water phase to form a water-in-oil emulsion. The effects of DS and the type of oil phase on emulsification properties were studied. It shows that when the DS is 1.91, the emulsification performance is the best. Compared with the emulsion stabilized by EM90, although the size of emulsion stabilized by trimethylsilyl pullulan is larger, it has higher viscosity and better stability. 数据和表 | 参考文献 | 相关文章 | 计量指标

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ATP生物荧光增幅法在化妆品微生物检测中的验证研究 Validation study of amplified ATP bioluminescence assay for microbial detection in cosmetics 翟磊,葛媛媛,崔生辉,刘吉泉,洪海军,Annemieke Masolijn,姚粟 2020 (11):  771-775.  doi: 10.3969/j.issn.1001-1803.2020.11.006 摘要 ( 344 )   HTML ( 5 )   PDF(904KB) ( 463 )   选取清洁类、护理类、美容修饰类6种化妆品和7株代表菌株,开展了ATP生物荧光增幅法与《化妆品安全技术规范》（2015年版）中菌落总数、霉菌和酵母菌检验方法的部分等效性研究。将代表菌株按照目标浓度10,5,1和0.1 CFU/g分别接种于6种化妆品,每个浓度重复检测5次,经Fisher exact test统计分析发现ATP生物荧光增幅法的检测限显著优于标准方法（p=0.000 1）。7株代表菌株在MTAT培养基中生长良好,ATP生物荧光增幅法检测人工污染样品结果均为阳性,表明该方法的专属性良好。选取3家不同的实验室,采用两种方法对相同产品进行比对检测,检测结果无统计学差异（p>0.05）,表明该方法的重现性良好。选取不同品牌TAT肉汤配制的富集培养基MTAT进行增菌,ATP检测结果均为阳性,表明该方法的耐用性良好。因此,ATP生物荧光增幅法与标准方法具有部分等效性。 Six kinds of cosmetics, including cleanser, care cosmetics and makeup categories, and seven representative microorganisms were selected to conduct the partial equivalence study between amplified ATP bioluminescence assay and the detection method of aerobic bacterial count and molds and yeast count in Safety and Technical Standard for Cosmetics （2015th Edition）. The seven representative microorganisms were inoculated into the six kinds of cosmetics at target concentrations of 10, 5, 1 and 0.1 CFU/g, respectively. Tests on each concentration were repeated five times. Fisher exact test statistical analysis show that the detection limit of amplified ATP bioluminescence assay is significantly better than that of the standard method （p=0.000 1）. Seven representative strains grew well in the MTAT medium, and the results of artificially contaminated samples detected by the amplified ATP bioluminescence assay were all positive, indicating that the method has good specificity. Three different laboratories were selected to compare the two methods using the same samples, and no statistical difference was found in the results, indicating the method is reproducible （p>0.05）. The enrichment media MTAT, prepared with selected brands of TAT base medium, were assessed using growth promotion, and their ATP test results were all positive, indicating that the method is has good durability. Therefore, the amplified ATP bioluminescence assay is partially equivalent to the standard method. 数据和表 | 参考文献 | 相关文章 | 计量指标

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疏水改性透明质酸的制备及性能 Preparation and properties of hydrophobically modified hyaluronic acid 石梦琳,刘力嘉,尚亚卓,刘洪来 2020 (11):  776-782.  doi: 10.3969/j.issn.1001-1803.2020.11.007 摘要 ( 478 )   HTML ( 21 )   PDF(1567KB) ( 839 )   通过化学反应将胆固醇（CHO）引入透明质酸（HA）的分子结构中,获得疏水改性透明质酸（HACHO）。利用核磁氢谱和红外光谱对合成产物结构进行了表征。使用透射电子显微镜（TEM）、荧光光谱以及流变仪等对HACHO的临界聚集浓度、在水中的自组装行为及流变行为等进行了研究。采用MTT法评价了HACHO的体外细胞毒性。在此基础上,将HACHO应用于制备双凝胶乳液,考察其稳定乳液的性能。结果表明,HACHO具有一定的界面活性,较好的生物相容性,且能在水相体系中形成较紧致的网络结构,能更好地稳定双凝胶乳液,在化妆品领域具有广阔的应用前景。 Cholesterol （CHO） was grafted onto the molecular structure of hyaluronic acid （HA） through a chemical reaction to obtain a modified product HACHO. 1H NMR and FT-IR were used to characterize the structure of the modified product. Transmission electron microscope （TEM）, fluorescence spectrum and rheometer were used to study the critical aggregation concentration, self-assembly behavior and rheological behavior of HACHO in water. The cell viability of the modified product HACHO was evaluated by the MTT assay. On this basis, HACHO was used to prepare bi-gel emulsion, and the stability of the emulsion was investigated. The results showed that, HACHO had interfacial activity and good biocompatibility, and could form a network structure in aqueous phase to stabilize the bi-gel emulsion. Therefore, HACHO showed a broad application prospect in the field of cosmetics. 数据和表 | 参考文献 | 相关文章 | 计量指标

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三七提取物的抗衰老功效性研究 Study on the anti-aging efficacy of Sanqi extract 高思宇,霍彤,李学涛,姚雪敏,陆俊聪,权强华 2020 (11):  783-787.  doi: 10.3969/j.issn.1001-1803.2020.11.008 摘要 ( 526 )   HTML ( 16 )   PDF(1413KB) ( 395 )   建立了衰老动物模型并对化妆品原料三七提取物的抗衰老功效进行评价。采用皮下注射D-半乳糖连续45 d得到衰老小鼠模型,在无毛区连续涂抹样品50 d。采用多功能皮肤分析仪对小鼠皮肤的肤色、色素及毛孔等指标进行测定。通过免疫组织化学染色对I型胶原蛋白（Col-I）、III型胶原蛋白（Col-III）与波形蛋白（VIM）进行观察。对皮肤组织匀浆进行总超氧化物歧化酶（T-SOD）、过氧化氢酶（CAT）、谷胱甘肽过氧化物酶（GSH-Px）及丙二醛（MDA）含量测定以评估样品处理后抗氧化能力的变化。结果表明,通过免疫组织化学染色可知4%三七软膏组可明显提高Col-I、Col-III与VIM的含量;三七软膏对T-SOD和GSH-Px的上调作用具有较好的剂量依赖效果。其中4%三七软膏组与空白基质组相比,T-SOD活力值增加了36.62%,CAT活力值增加了20.39%,GSH-Px活力值增加了68.77%。 An aging animal model was established and the anti-aging effects of Sanqi extract as a cosmetic ingredient were evaluated. D-galactose was injected subcutaneously for 45 days to obtain an aging mouse model. The samples were continuously applied to the hairless area for 50 days. Multifunctional skin analyzer was used to measure the skin color, pigment, and pores of the mouse skin. Collagen I （Col-I）, Collagen III （Col-III） and vimentin （VIM） were evaluated by immunohistochemical staining. Total superoxide dismutase （T-SOD）, catalase （CAT）, glutathione peroxidase （GSH-Px） and malondialdehyde （MDA） in skin tissue homogenates were measured to evaluate the changes in antioxidant capacity after sample treatment. The results showed that the ointment containing 4% Sanqi extract could significantly increase the content of Col-I, Col-III and VIM by immunohistochemical staining. Sanqi ointment had a good dosage-dependent effect on the up-regulation of T-SOD and GSH-Px. Compared with the blank matrix group, the T-SOD activity was increased by 36.62%, the CAT activity was increased by 20.39%, and the GSH-Px activity was increased by 68.77% after treatment with the ointment containing 4% Sanqi extract. 数据和表 | 参考文献 | 相关文章 | 计量指标

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滇黄精提取物成分与活性测定及细胞毒性评价 Determination of components and activity of extractions of Polygonatum kingianum and evaluation of its cytotoxicity 施扬,王力川,马占林,周戟,陈军文,赵明 2020 (11):  788-792.  doi: 10.3969/j.issn.1001-1803.2020.11.009 摘要 ( 522 )   HTML ( 15 )   PDF(1236KB) ( 868 )   制备滇黄精提取物,测定多糖、多酚、皂苷和黄酮类成分含量,以及抗氧化能力和酪氨酸酶抑制活性,并采用细胞试验研究提取物安全性,评价黄精提取物在日化产品中的应用潜力。结果表明:干制、蒸制和酒制滇黄精提取物总多糖、多酚、皂苷和黄酮含量分别为39.68%~56.33%,0.31%~4.11%,4.10%~8.54%,0.14%~0.47%;三种提取物都具有一定的还原力、较高的羟自由基和DPPH自由基清除率以及酪氨酸酶抑制活性,并且同一浓度下酒制黄精提取物活性显著高于另外两种提取物（P<0.05）。角质形成细胞和成纤维细胞活性测定发现,0.2%含量内的酒制黄精提取物无细胞毒性。综上,黄精提取物尤其是酒制滇黄精提取物含有多糖、皂苷等活性成分,具有抗氧化与酪氨酸酶抑制活性,且无细胞毒性,在日化产品中具有重要的应用价值。 Extractions of Polygonatum kingianum were prepared, and the contents of polysaccharide, polyphenols, saponins, flavonoids, as well as the antioxidant activity and tyrosinase inhibitory activity were determined. The safety of the extraction was studied by cell test, and its application potential in daily chemical products was evaluated. The results show that the contents of total polysaccharides, polyphenols, saponins, flavonoids of dried, steamed and alcoholic extractions of P. kingianum were 39.68%-56.33%, 0.31%-4.11%, 4.10%-8.54%, 0.14%-0.47%, respectively. The three kinds of extractions show a certain reducing power, high scavenging rate of hydroxyl radical and DPPH free radical, and tyrosinase inhibitory activity. With the same concentration, the activity of the alcoholic extraction of P. kingianum is significantly higher than the other two extractions （P<0.05）. The activities of keratinocytes and fibroblast cells reveal that 0.2% of alcoholic extraction of P. kingianum is non-cytotoxic. Together, the extraction of P. kingianum, especially the alcoholic extraction, are rich in polysaccharides, saponins and other active compounds, and show antioxidant and tyrosinase inhibitory activities without cytotoxicity. It has an important application value in daily chemical products. 数据和表 | 参考文献 | 相关文章 | 计量指标

专论与综述

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化妆品经皮渗透研究进展——评价方法及促渗技术 Progress in research of skin permeability of cosmetics Evaluation method and enhancement technology 杨曼丽,周明月,胡雪情,陈风,何聪芬,贾焱 2020 (11):  793-798.  doi: 10.3969/j.issn.1001-1803.2020.11.010 摘要 ( 1556 )   HTML ( 55 )   PDF(893KB) ( 1633 )   对于化妆品中应用的经皮递送系统,列举常见的促渗方法,包括化学促渗技术、纳米技术（纳米乳液、纳米晶体、脂质体、类脂囊泡、微胶粒等）、物理促渗技术（离子导入、超声导入、微针）以及生物促渗技术等。对化妆品体外透皮吸收试验方法（体外扩散池法、数学模型、三维皮肤模型、液质联用、拉曼光谱）进行了简单介绍,并对化妆品经皮渗透方法进行了展望。 For the transdermal delivery system used in cosmetics, the common methods for promoting penetration have been listed, including chemical permeation-enhancing techniques, nanotechnology （nanoemulsions, nanocrystals, liposomes, niosomes, micelles, etc.）, physical permeation-enhancing techniques （iontophoresis, ultrasonic introduction, and microneedle） and biological permeability-promoting technology. The testing methods of transdermal absorption of cosmetics in vitro （in-vitro diffusion cell method, mathematical model, three-dimensional skin model, LC-MS, and Raman spectroscopy） have been briefly introduced, and the future transdermal penetration methods of cosmetics have been prospected. 参考文献 | 相关文章 | 计量指标

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基于图形元素视觉创意的洁面皂产品外观包装设计 Design of appearance and package of facial soap products based on visual creativity of graphic elements 王晓固,刘康 2020 (11):  799-803.  doi: 10.3969/j.issn.1001-1803.2020.11.011 摘要 ( 226 )   HTML ( 8 )   PDF(924KB) ( 484 )   为了提升洁面皂产品外观包装设计的创意性,让设计呈现个性化与不可替代性,围绕基于图形元素视觉创意的洁面皂产品外观包装设计问题进行分析。分析图形元素可知,图形元素属于洁面皂产品包装设计中独一无二的特征描述;洁面皂外观包装中所用图形创意在现代包装设计中需要遵循准确性、个性化、艺术性、局限性4个原则;基于图形元素视觉创意的洁面皂产品外观包装设计可从图形同构、正负图形、异变异影、文字图形、文字变形、文字组合、传统艺术相融合以及合理用色等方面出发,实现洁面皂产品外观包装优秀设计。 In order to enhance the creativity of design of the appearance and package of facial soap products and make the design personalized and irreplaceable, we have discussed this issue based on the visual creativity of graphic elements. Through the analysis of graphic elements, it can be seen that the graphic elements belong to the unique feature description in the packaging design of soap products; in modern packaging design, the graphic creativity used in the appearance packaging of soaps should follow four principles: accuracy, individuation, artistry and limitation; based on the visual creativity of graphic elements, the appearance packaging design of soap products can be realized from the following aspects: graphic isomorphism, positive and negative graphics, variant shadows, text graphics, text deformation, text combination, integration of traditional art and reasonable color use. 数据和表 | 参考文献 | 相关文章 | 计量指标

分析与检测

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超高效液相色谱法测定化妆品中11种香豆素类化合物及质谱确证 Simultaneous determination of eleven coumarins in cosmetics by ultra high performance liquid chromatography and verification by liquid chromatography-tandem mass spectrometry 陈卫,张斌,陈丽波,钱叶飞,赵琪,贾昌平 2020 (11):  804-808.  doi: 10.3969/j.issn.1001-1803.2020.11.012 摘要 ( 335 )   HTML ( 7 )   PDF(1051KB) ( 766 )   建立了同时测定化妆品中11种香豆素类化合物（8-羟基补骨脂素、补骨脂素、6-甲基香豆素、异补骨脂素、8-甲氧基补骨脂素、5-甲氧基补骨脂素、补骨脂二氢黄酮、新补骨脂异黄酮、三甲沙林、欧前胡素和异欧前胡素）的超高效液相色谱方法及液相色谱-串联质谱确证方法。样品用甲醇超声提取20 min,离心后取上清液经微孔滤膜过滤后测定。采用ACQUITY UPLC HSS T3色谱柱（2.1 mm×50 mm,1.8 μm）,以乙腈-水为流动相进行梯度洗脱,流速为0.3 mL/min,柱温为30 ℃,检测波长为246和278 nm。以超高效液相色谱法的结果进行定性筛查,并采用标准曲线法定量,以液相色谱-串联质谱法的结果进行确证。结果表明,11种香豆素类化合物的线性范围均为1.0~10 mg/L,相关系数均大于0.999 7。方法检出限为0.1~0.6 mg/kg。在低、中、高3种加标水平下,平均回收率为95.3%~110.0%,RSD为0.4%~2.6%。该方法简便、快速、准确,适用于化妆品中11种香豆素类化合物的同时检测。 A method for the simultaneous determination of eleven coumarins （8-hydroxypsoralen, psoralen, 6-methylcoumarin, isopsoralen, 8-methoxypsoralen, 5-methoxypsoralen, bavachin, neobavaisoflavone, trioxsalen, imperatorin and isoimperatorin） in cosmetics by ultra high performance liquid chromatography verification by liquid chromatography-tandem mass spectrometry was established. The cosmetic samples were ultrasonically extracted with methanol for 20 min, centrifuged, and the supernatant was filtered through a microporous membrane for determination. An ACQUITY UPLC HSS T3 chromatographic columns （2.1 mm×50 mm, 1.8 μm） was used for gradient elution at a flow rate of 0.3 mL/min with acetonitrile-water as the mobile phases. The wavelengths of detection were 246 and 278 nm. The column temperature was set at 30 ℃. The results of ultra high performance liquid chromatography were used for qualitative screening, 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 the linear ranges of the eleven coumarins were 0.1-10 mg/L, and the correlation coefficients were all greater than 0.999 7. The detection limits are 0.1-0.6 mg/kg. The average recoveries are 95.3%-110.0% with RSDs of 0.4%-2.6% at low, medium and high spiked levels. The method is simple, rapid and accurate for the simultaneous determination of eleven coumarins in cosmetics. 数据和表 | 参考文献 | 相关文章 | 计量指标

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高效液相色谱法测定口腔清洁护理用品中o-伞花烃-5-醇含量的研究 Research on the determination of o-cymene-5-ol in oral care and cleansing products by HPLC 施裔磊 2020 (11):  809-814.  doi: 10.3969/j.issn.1001-1803.2020.11.013 摘要 ( 402 )   HTML ( 8 )   PDF(1187KB) ( 521 )   建立用高效液相色谱法测定牙膏、漱口水等口腔清洁护理用品中o-伞花烃-5-醇含量的方法。样品用50%甲醇水溶液溶解,经磁力搅拌、超声提取、离心分离及过滤处理,以Dionex AcclaimTM 120型C18为色谱柱,乙腈-10 mmol/L磷酸二氢钾为流动相进行梯度洗脱,流量为1.5 mL/min,柱温为30 ℃,采用二极管阵列检测器进行检测,检测波长为279 nm,外标法定量。研究结果表明,o-伞花烃-5-醇在1.00~15.0 mg/L的质量浓度范围内与其峰面积具有良好的线性关系,R2=0.999 9,方法的检出限为20 mg/kg,定量限为60 mg/kg,样品加标回收率为96.3%~101.4%,测定结果的相对标准偏差为0.41%~1.63% （n=6）。该方法具有操作简便、灵敏度高、重现性好等特点,适用于口腔护理产品中o-伞花烃-5-醇的定性定量分析。 A reversed-phase high performance liquid chromatographic method was developed for the determination of o-cymene-5-ol in oral care and cleansing products such as toothpastes and mouthwash. Samples were extracted by 50% methanol aqueous solution, and preprocessed by magnetic stirring, ultrasonic extraction, centrifugation and filtration. Dionex Acclaim TM 120 C18 was used as a chromatographic column and acetonitrile-10 mmol/L monopotassium phosphate as mobile phase for gradient elution. The flow rate was 1.5 mL/min, and the column temperature was 30 ℃. The detection was carried out by a diode array detector with the wavelength of 279 nm. The external standard method was used for quantitative analysis. The mass concentration of o-cymene-5-ol in the range of 1.00-15.0 mg/L shows a good linear relationship with the peak area. The correlation coefficient is 0.999 9, the detection limit is 20 mg/kg and the quantitative limit is 60 mg/kg. The recovery rate is 96.3%-101.4%, and the relative standard deviation is 0.41%-1.63% （n=6） . The method is simple, sensitive and reproducible. It is suitable for the determination of o-cymene-5-ol in oral care and cleansing products. 数据和表 | 参考文献 | 相关文章 | 计量指标