Determination of alpha-hydroxy acids in cosmetic products by high-performance liquid chromatography with a narrow-bore column

This paper reports the results of a study carried out to develop a simple, rapid and sensitive method for the separation, identification and quantitative measurement of alpha-hydroxy acids in commercial cosmetics using high-performance liquid chromatography (HPLC). This method is successfully applied to the simultaneous identification and quantitative determination of glycolic, lactic, malic, tartaric and citric acids employing a reversed phase narrow-bore column under isocratic condition and UV detection. The method is validated by determining the precision of replicate analyses and accuracy by analyzing samples with and without adding know amount of the alpha-hydroxy acids. The procedure is suitable for routine analyses of commercial cosmetics.     

Comparative effectiveness of α-hydroxy acids on skin properties

A number of α-hydroxy acids, including glycolic, lactic ( l (+) and d (–) forms) citric, hydroxybutyric and malic acids, were evaluated for their effects on various skin properties at concentrations of 0.5–1.15 m . The acids were evaluated for their stinging potential on sensitive skin, the ability to increase skin cell renewal, and their ability to improve moisture content and reduce lines and wrinkles over a six-week period. Results indicated that lactic l (+) and glycolic were the most effective acids when tested at equimolar concentrations. Both materials were less irritating than the d (–) lactic acid form and the other acids tested. Even though with long-term use both d (–) and l (+) lactic acid and glycolic acid produced comparative improvements in skin hydration and lines and wrinkle improvement, the l (+) form of lactic acid did so with fewer consumer complaints than any of the other acids tested. When the concentration of lactic and glycolic acids was increased to more than 1.5 m a greater difference in irritation potential was observed with respect to stinging, with the l (+) form of lactic acid being less irritating than glycolic acid and the d (–) form. Our results suggest that l (+) and d (–) lactic acid and glycolic acid are the two most effective materials for developing α-hydroxy acid products. Lactic acid has a slight technical advantage over glycolic acid. Both l (+) and the d (–) forms are better moisturizers when fully or partially neutralized. Moreover the l (+) form is also less irritating than d (–) and glycolic acid. Other acids such as citric, malic, and hydroxybutyric acids appear to be less effective materials but may be useful additions to lactic or glycolic acid mixes.     

HPLC determination of thioglycolic acid and other aliphatic thiols in cosmetic formulations using ethacrynic acid as precolumn derivatization reagent

Limits imposed on the usage of thioglycolic acid, its salts and esters in cosmetic formulations require selective and sensitive analytical methods for their determination. In this study a convenient and reliable method based on high-performance liquid chromatography (HPLC) has been developed. The method involves a precolumn reaction of the thiol compounds with ethacrynic acid to give thiol adducts which can be separated by reversed-phase liquid chromatography and detected at λ= 273 nm.
The derivatization reaction proved to be quantitative under mild conditions (20 min at pH 7.4 and room temperature) and the chromatographic conditions allowed thioglycolic acid, glyceryl monothioglycolate, thiolactic acid, and thioglycolic acid ethyl ester to be discriminated.
The proposed method was successfully applied to the analysis of commercial cosmetic formulations containing thioglycolic acid and glyceryl monothioglycolate, fulfilling the requirements of a general and selective method for the analysis of aliphatic thiols in cosmetics.     

化妆品中柠檬酸检测能力验证结果分析

目的考察相关实验室检测化妆品中柠檬酸的技术能力和水平,促进参加实验室对该类项目检验能力的提高。方法样品通过均匀性和稳定性评价后,采用随机单盲方式分配至参与能力验证(proficiency testing,PT)的实验室。统计各参加实验室的测定结果,进行稳健统计分析,通过Z比分数评价实验室检测能力。结果制备的200瓶样品均匀性符合要求且在整个计划周期内保持稳定,满足能力验证计划要求。从参加的31家的结果来看,共有27家满意,满意率为87.1%。结论化妆品中柠檬酸的检测水平总体良好,个别实验室检测能力有待提高。     

Analysis of diglycolic acid in food packaging,over the counter products,direct additive carboxymethyl cellulose,and retail foods

ABSTRACT

Carboxymethyl cellulose (i.e. CMC or cellulose gum) is used as a direct additive for foods and drugs to change texture and act as a binder. CMC can also be a fluid absorbent used in food packaging and food contact materials. CMC and other carboxymethyl starches are synthesised by condensing glycolic acid with monochloroacetic acid. Diglycolic acid (DGA) is a byproduct produced by this condensation which cannot be completely removed. Currently, there are no analytical methods to accurately detect and quantify DGA in foods and food packaging materials. A method using a methanol/water extraction coupled with weak anion exchange solid phase extraction cleanup for more complex matrices was developed. A novel LC-MS/MS method was used to determine the DGA concentration in food contact materials, food grade direct additive CMC, and foods containing CMC. This paper will discuss the development of a new method for the preparation and cleanup of various food matrices and LC-MS/MS analysis for the presence of DGA.     

QuEChERS-超高效液相色谱-串联质谱法快速测定化妆品中糖皮质激素类药物

目的建立QuEChERS-超高效液相色谱-串联质谱法快速测定化妆品中16种糖皮质激素类药物的检测方法。方法样品经1%(V/V)甲酸-乙腈提取,加入氯化钠进行盐析,提取液经C₁₈50 mg、N-丙基乙二胺(primary secondary amine,PSA)100 mg、MgSO₄150 mg净化,采用Thermo Acclaim RSLC 120 C₁₈(2.1 mm×100 mm,2.2μm)进行分离,电喷雾正离子多反应监测扫描(multiple reaction monitoring,MRM)模式下进行测定,外标法定量。结果16种糖皮质激素在线性范围1~100 ng/mL内线性良好,相关系数r²在0.991~0.999之间,方法定量限为10μg/kg,16种糖皮质激素平均回收率在76.5%~109.3%之间,相对标准偏差为0.77%~2.41%。结论该方法操作简单、净化效果好、灵敏度、准确度和精密度均符合多残留检测技术要求,解决了化妆品中糖皮质激素类药物检测提取过程过于繁琐的问题,可为化妆品检测提供更方便、更快捷的检测方法支持。     

Combined retinol-lactose-glycolic acid effects on photoaged skin: a double-blind placebo-controlled study

The objective of this study was to assess the efficacy of the combination of retinol, lactose and glycolic acid applied topically on photodamaged skin. Forty female volunteers were enrolled in a double-blind, randomized placebo-controlled clinical study. A cream containing retinol, lactose and glycolic acid was applied on one side of the face and a placebo cream on the other side, twice daily for 12 weeks. Skin photoageing signs were assessed clinically, whereas skin microrelief and moisturization were measured instrumentally. Both the clinical assessment and the objective instrumental measurements revealed that the active-treated side was significantly improved at the end of the study compared with baseline and control-treated side. In conclusion, our results demonstrate that topical application of a combination of retinol, lactose and glycolic acid has significantly improved the appearance of photodamaged skin.     

Determination of phthalate esters in cosmetics by gas chromatography with flame ionization detection and mass spectrometric detection

A gas chromatography coupled with flame ionization detection (GC-FID) and mass spectrometric detection (MSD) method was developed to determine the six kinds of phthalate esters [dimethyl phthalate (DMP), diethyl phthalate (DEP), di-n-butyl phthalate (DBP), benzyl butyl phthalate (BBP), di(2-ethylhexyl) phthalate (DEHP) and di-n-octyl phthalate (DOP)] in cosmetics (solid, cream and liquid cosmetics). The cosmetics were extracted with methanol by ultrasonic and then separated with high-speed centrifugation. The upper clear layer was dried and filtered through a 0.45 mum pore diameter filter. The filtrate was injected into GC-FID/GC-MS for detection. GC-FID chromatogram was applied for qualitative analysis, external standard method was used for quantitative analysis. Confirmation of phthalate presence was undertaken by GC-EI-MS. The recovery range of all phthalates were between 92.0 and 110.0% with relative standard deviations between 1.95 and 5.92%. The low detection limits of the method were: 0.1 ng for DMP, DEP, DBP and BBP, 0.5 ng for DEHP and DOP. The method had advantages of high precision and sensitivity, simplicity of pretreatment. The method can be used to test the six kinds of phthalate esters in cosmetics.     

电感耦合等离子体发射光谱法测定网络销售豆制品零食中的硼酸

目的 采用超声萃取,建立电感耦合等离子体发射光谱仪测定网络销售豆制品零食中硼酸含量的方法。方法 以2%硫酸水溶液为提取剂,10%三氯乙酸为沉淀剂,超声提取样品中硼酸,外标法定量硼酸。结果 硼在249.678 nm波长下,0.01~1.00 mg/L范围内与信号强度呈良好线性关系,相关系数为0.99967,检出限(以硼酸计)为0.006 mg/kg。豆制品零食样品中3水平的加标回收率为95.7%~105%,RSD%为0.2%~1.8%。采用本文建立的方法对140批次的网络销售豆制品零食中硼酸的含量进行检测,含量范围为2.22~168 mg/kg,且82.1%的网络销售豆制品零食中的硼酸含量小于50 mg/kg。结论 该方法前处理简单、检测速度快,可用于豆制品零食类样品中硼酸的检测。     

曲酸及其衍生物的研究进展

曲酸作为一种新型的食品和化妆品添加剂,吸引了众多食品化学、医药、生物学家的研究兴趣。文中介绍了曲酸的结构、化学性质,并对曲酸生产的菌株、发酵方法、抗菌防腐、护色保鲜及其安全性能作了综述。     

食用植物油酸值检测研究进展

酸值是衡量食用植物油中游离脂肪酸（free fatty acid, FFA）含量的指标,也是其重要的氧化和质量指标。目前食用油酸值测定方法中最常用的是滴定法,该方法简单、易行,对多数油脂的检测是有效的,但对酸值较低、颜色较深或存在除FFA外干扰成分的油脂检测误差较大,光谱法、电化学法、比色法、色谱法等仪器分析方法可以作为其替代方法,且仪器分析方法具有较好的灵敏度、准确性。为了进一步拓展和创新食用植物油酸值检测的技术与方法,实现各种植物油酸值的快速准确检测,分析比较了食用植物油FFA的产生途径、酸值检测方法的特点、现状,以期为酸值检测方法的改进及新方法的建立提供参考。     

现行黄曲霉毒素液相色谱检测法的比较与评价

目的 综合评价检测黄曲霉毒素的几种现行液相色谱-荧光法。方法 采用均质(涡旋)、超声辅助液液萃取技术对样品中的黄曲霉毒素进行提取, 免疫亲和柱和多功能柱净化。并采用不同的检测技术[三氟乙酸(TFA)柱前衍生法、光化学柱后衍生法、碘和溴柱后衍生法、大体积流动池直接检测及光化学柱后衍生串联大体积流动池]对玉米质控样品中黄曲霉毒素进行了分析。结果 各方法的检测结果均较理想, 可满足常规样品的检测要求。结论 超高压液相色谱-大体积流动池检测法在有效提高工作效率的同时, 大量减少了有毒有害试剂的使用量, 且具有最高的检测灵敏度, 可满足GB 2761-2011中对各类样品中黄曲霉毒素的限量要求。采用乙腈-水或甲醇-水体系均能达到较好提取黄曲霉毒素的目的。免疫亲和柱的净化效果较多功能柱好。     

生物法制备乙醇酸的研究

目的:对氧化葡萄糖酸杆菌生物转化乙二醇生产乙醇酸的工艺进行研究.方法:首先采用单因素试验优化了氧化葡萄糖酸杆菌生物转化乙二醇生成乙醇酸的工艺,在此基础上通过正交试验对转化工艺进行了进一步探讨.结果:氧化葡萄糖酸杆菌生物转化乙二醇生成乙醇酸的最优工艺为12.6%静息细胞、5.6%乙二醇维持pH5.84转化48h,乙二醇单体转化率可达60.886%.结论:应用氧化葡萄糖酸杆菌生物转化乙二醇生产乙醇酸的工艺的切实可行.     

燕窝中唾液酸的DAD/FLD串联HPLC测定方法研究

建立燕窝中唾液酸的柱前衍生二极管阵列/ 荧光检测器(DAD/FLD)串联的反相高效液相色谱检测方法。用硫酸氢钠溶液水解样品,以邻苯二氨盐酸盐为衍生化试剂,采用C18 柱分离,四氢呋喃溶液(含体积分数0.5%磷酸和体积分数0.15% 正丁胺)- 乙腈为流动相等度洗脱,流速1.0mL/min,二极管阵列检测波长230nm,荧光激发波长(Ex) 230nm,发射波长(Em) 425nm。结果表明,唾液酸在0.1～750μg/mL 范围内线性良好(r ＞ 0.9990),20min内完全分离,回收率在85.03%～97.14% 之间。检出限0.2μg/mL(DAD),0.005μg/mL (FLD),FLD 检出限比DAD低两个数量级且杂峰少,在DAD 检出限以上的相同浓度下,DAD 比FLD 更灵敏。本方法具有灵敏度高,重复性好,分析速度快等特点,可准确测定燕窝等样品中唾液酸含量。     

Al3+荧光增敏快速检测酸奶和乳酸菌饮料中的胭脂虫红酸（英文）

研究溶剂、浓度、pH值以及金属离子对胭脂虫红酸荧光性能的影响,表明胭脂虫红酸在pH 4且其物质的量浓度为2.0×10^-4 mol/L的水溶液中荧光最强;而胭脂虫红酸对金属离子选择性识别的结果显示,Al^3+能使胭脂虫红酸的荧光强度显著增强从而提高检测的灵敏度。以Al^3+(2.0×10^-3 mol/L)为标准溶液检测样品中胭脂虫红酸含量时,胭脂虫红酸的物质的量浓度在1.0×10^-5~8.0×10^-5 mol/L范围内与其荧光强度呈良好的线性关系,检测限为5.0×10^-6 mol/L。实际应用结果表明,用荧光法检测不同酸奶和乳酸菌饮料中添加的胭脂虫红酸的含量,样品回收率在96.6%~110.5%之间,相对标准偏差小于5.9%。本研究为快速、有效、定量地检测食品中的胭脂虫红酸提供了一种有效的方法。     

脂溶性阿魏酸衍生物合成研究进展

阿魏酸作为一种天然抗氧化剂,已广泛用于食品、化妆品、医药等业。该文综述目前国内外合成脂溶性阿魏酸衍生物方法,为阿魏酸开发应用提供基础。     

Simultaneous determination of some ultraviolet-absorbing chemicals in sunscreen cosmetics using a high-performance liquid chromatography method

A method of gradient elution high-performance liquid chromatography (HPLC) for simultaneous determination of 11 different ultraviolet-absorbing chemicals of phenylbenzlmldazole sulphonic acid, 4-aminobenzoic acid, benzophenone-4, benzophenone-3, isoamyl p-methoxycinnamate, 4-methylbenzylidene camphor, octocrylene, ethylhexyl methoxycinnamate, homosalate, ethylhexyl salicylate, methylene bis-benzotriazolyl tetramethylbutyl phenol was developed for the application to sunscreen cosmetic products. In this study, an Agilent SB-C18 analytical column (250 × 4.6 mm, 5 μm) was utilized and methanol, tetrahydrofuran and perchloric acid aqueous solution (0.2 mL HClO(4) + 300 mL H(2)O) were used for gradient elution at a total flow rate of 1.0 mL min(-1). The optimum conditions for 11 different ultraviolet-absorbing chemicals analyses were investigated. All calibration curves showed good linear regression with UV detection (311 nm) within test ranges. The correlation coefficients were better than 0.999 in all cases. The assay was simple, selective, convenient and reproducible and is suitable for the determination of ultraviolet-absorbing chemicals in commercial sunscreen cosmetic products. The use frequency of 11 different ultraviolet absorbents in 100 sunscreen cosmetics was investigated and statistically analysed. The ultraviolet absorbent of maximum use frequency was ethylhexyl methoxycinnamate.     

液相色谱法与氨基酸分析法测定食品中甘氨酸的比较研究

建立对食品中游离甘氨酸经提取、净化等处理后,邻苯二甲醛衍生,经高效液相色谱测定分析,并将该方法与氨基酸分析仪测定甘氨酸的方法进行比较研究。通过对市售的液体乳、含乳饮料(品)类和植物蛋白饮料(品)类中游离甘氨酸分别应用两种方法进行测定,结果表明,氨基酸分析仪法测定甘氨酸具有测定结果稳定准确、检出限低和操作简单的特点,而液相色谱法(荧光检测器)测定甘氨酸检测时间快,检出限也能满足常规检测的需要,因此,在实际应用中,两种方法均可采用,可作为互相验证的方法。     

透明质酸的制备及其应用的研究进展

透明质酸(hyaluronic acid,HA)作为一种线性黏多糖,其在人体内分布广泛,发挥着重要的生理功能作用,由于其独特的理化性质和生理功能,在保健品、化妆品、医药等方面应用广泛.2021年我国批准HA作为新资源食品原料,了解其制备及分离纯化方法对推动其产业化发展很有必要,本文综述了HA的生理功能、不同来源HA的制...     

Evaluation of 'nuez de barinas' (caryodendron orinocense) oil for possible use in cosmetic

Caryodendron orinocense, Karst., is a tree that grows along the eastern base of the Andes mountains in Venezuela, Ecuador, and Colombia. It is known in Venezuela as 'Nuez de Barinas, nuez or nogal de Barquisimeto' and in other countries as 'inchi', 'taque', 'abay' or 'palo de nuez'. The oil extracted from the 'nuts' (seeds) is edible. The objective of this study was to assess the potential use of the oil extracted from the seeds in cosmetics. The organoleptic characteristics, some physical (viscosity, specific density, extensibility, UV absorbance), and chemical (fatty acid profile, titratable acidity, saponification index, unsaponifiable matter and peroxide value) characteristics, were determined by official methods. The results show a high polyunsaturated fatty acid content (75.13%) and good physical, chemical and toxicological characteristics appropriate for use in cosmetics. It was concluded that the Caryodendron oil should be useful in cosmetic formulations.