双水相萃取快速提取测定化妆品中有机污染物与添加剂的方法研究

发布时间：2018-06-09 00:42

本文选题：化妆品 + 双水相体系　；参考：《烟台大学》2017年硕士论文

【摘要】：随着人们生活水平与健康意识的提高,各类化妆品中可能存在的有机污染物与化学添加物质(如:抗氧化剂、抗生素、抗紫外剂等)的种类与含量引起了消费者的重视,与之相关的检测技术问题也受到研究者的关注。目前用于各种化合物检测的仪器已经能够满足检测的要求,由于化妆品样品基体的复杂性,因此在检测过程中样品前处理技术是制约化合物检测的主要因素。论文对化妆品中六种苯系物(BTEX)、两种抗氧化剂(BHA、BHT)、磺胺类药物和四环素类药物的现有的前处理方法及检测方法进行了综述,采用双水相基质去除法作为样品前处理技术高效提取化妆品中的目标物质,结合气相色谱-质谱联用(GC-MS)和高效液相色谱(HPLC)实现了目标物质的快速、准确测定。论文主要分为五个部分:第一部分:阐述化妆品样品常用的前处理方法,并说明了本文的研究意义和主要研究内容。第二部分:基于异丙醇-(NH_4)2SO_4-H_2O双水相样品的预处理的方法,运用气相色谱-质谱联用(GC-MS)建立了一种环境友好型检测化妆品样品中六种苯系物(苯、甲苯、乙苯、对二甲苯、间二甲苯和邻二甲苯)的方法。实验考察了双水相的形成条件,并探讨了不同含水量的化妆品样品对双水相萃取率的影响。结果显示,与有机溶剂乙腈和乙醇相比,异丙醇破乳作用最好;异丙醇和水的体积比对化妆品中六种苯系物的提取率有影响,当异丙醇与水的体积比大约为2:3时,因为化妆品中的苯系物与异丙醇能够充分接触,所以六种苯系物的提取率较高。根据本方法对化妆品样品进行测定,回收率为81.1~98.2%,检出限为1.1~3.9ng/g。第三部分:用异丙醇-NaCl-H_2O双水相体系基质去除法高效提取化妆品样品中的抗氧化剂(BHA、BHT),结合气相色谱-质谱联用(GC-MS)实现了对化妆品样品中两种抗氧化剂的快速准确测定。实验考察了有机萃取溶剂、无机盐、净化剂及化妆品的含水量对BHA和BHT的萃取影响。结果表明实验中选用异丙醇破乳效果最好;体积分数约为40%的异丙醇水溶液为提取液,然后再加入NaCl形成双水相体系,抗氧化剂进入双水相上相实现BHA和BHT的高效萃取,此时化妆品中BHA和BHT的萃取效率最高。本方法用于检测多种市售的化妆品样品中BHA和BHT,均得到了满意的结果。测定回收率为84.1~96.5%,相对标准偏差RSD为2.11~4.03%。步骤简单、可靠,可很好地应用于化妆品中BHA和BHT的快速检测。第四部分:应用双水相技术进行样品预处理,以HPLC为检测手段,建立了化妆品中四种磺胺类化合物(SAs:磺胺噻唑(ST),磺胺甲基嘧啶(SM1),磺胺二甲基嘧啶(SM2),磺胺氯哒嗪(SCP))的快速分析方法。配制磺胺类化合物的标准溶液时,实验发现用50%的乙腈水溶液作为标准稀释液时,四种磺胺类药物峰形最好,回收率最高。实验考察了双水相的形成条件及不同含水量的化妆品对磺胺类化合物萃取率的影响,结果表明,选择提取溶剂为约30%甲醇水溶液,无机盐为磷酸氢二钾时,四种磺胺类药物的萃取率最高。按照实验方法对多种化妆品进行检测,SAs的回收率范围为81.1~99.5%,相对标准偏差RSD为2.01~4.09%。第五部分:以甲醇-磷酸氢二钾-水双水相体系高效提取化妆品样品中的四环素类药物(TCs:四环素、土霉素和金霉素),结合高效液相色谱(HPLC)技术实现了对化妆品样品中的四环素类药物的快速准确检测。实验考察了双水相的形成条件对四环素类化合物萃取率的影响,结果表明,提取溶剂为约30%甲醇时,甲醇与化妆品中的四环素类化合物接触更充分,从而萃取化妆品中的四环素类药物,上相中加入净化剂PSA和C_(18)吸附杂质,目的是高效提取化妆品中的三种四环素类物质。本方法应用于化妆品中的四环素类化合物的提取测定,回收率为87.1~98.1%,检出限分别为14.4、18.1和19.1 ng/g。
[Abstract]:With the improvement of people's living standards and awareness of health, the types and contents of organic pollutants and chemical additives (such as antioxidants, antibiotics, anti ultraviolet agents, etc.) in all kinds of cosmetics have aroused the attention of consumers, and the related detection technology problems have also been paid attention to by the researchers. The measuring instruments have been able to meet the requirements of testing. Because of the complexity of the cosmetic sample matrix, the preprocessing technology is the main factor restricting the detection of compounds. The present preprocessing of six kinds of benzene series (BTEX), two kinds of antioxidants (BHT), sulfonamides and tetracycline drugs in cosmetics is presented in this paper. The method and detection methods are reviewed. The target substances in cosmetics are extracted by using the biaqueous matrix removal method as sample pretreatment technology. The target substance is realized quickly and accurately by gas chromatography-mass spectrometry (GC-MS) and high performance liquid chromatography (HPLC). The thesis is divided into five parts: the first part: expatiate on makeup The research significance and main contents of this paper are described in common use. The second part: Based on the pretreatment method of isopropanol - (NH_4) 2SO_4-H_2O biaqueous sample, the gas chromatography-mass spectrometry (GC-MS) is used to establish a environmentally friendly detection of six benzene compounds (benzene, toluene, ethylbenzene) in cosmetics samples. The formation conditions of dimethylbenzene, dimethylbenzene and o-xylene were investigated. The effects of different water content on the extraction rate of water phase were investigated. The results showed that the demulsification of isopropanol was the best compared with the organic solvent acetonitrile and ethanol, and the volume ratio of isopropanol and water to six kinds of benzene in cosmetics. When the ratio of the volume ratio of isopropanol to water is about 2:3, the extraction rate of the six kinds of benzene series is high, because the benzene series in the cosmetics and isopropanol are fully exposed. According to this method, the recovery rate of the cosmetics is 81.1~98.2% and the detection limit is 1.1~3.9ng/g. third: isopropanol -NaCl-H_2 The O double aqueous phase system matrix removal method was used to efficiently extract the antioxidants (BHA, BHT) in cosmetic samples and the rapid and accurate determination of two kinds of antioxidants in cosmetics samples by gas chromatography mass spectrometry (GC-MS). The effects of organic extraction solvent, inorganic salt, purifier and cosmetics on the extraction of BHA and BHT were investigated. The results show that isopropanol has the best demulsification effect in the experiment, and the aqueous solution of isopropanol with a volume fraction of about 40% is the extraction solution, and then NaCl is added to form a dual aqueous phase system, and the antioxidants enter the two aqueous phase to achieve high efficiency extraction of BHA and BHT. At this time, the extraction efficiency of BHA and BHT in cosmetics is the highest. This method is used to detect many kinds of market. The results of BHA and BHT in cosmetics samples are satisfactory. The recovery rate is 84.1~96.5%, the relative standard deviation RSD is 2.11~4.03%. step simple and reliable. It can be well applied to the rapid detection of BHA and BHT in cosmetics. The fourth part: using the biaqueous phase technology to pretreat samples and establish the cosmetics with HPLC as the testing method. Four sulfonamides (SAs: sulfathiazide (ST), sulfamethazine (SM1), sulfamethazine (SM2) and sulfonamidazine (SCP) are fast analyzed. When the standard solution of sulfonamides is prepared, it is found that when 50% acetonitrile aqueous solution is used as standard diluent, four sulfonamides have the best peak shape and the highest recovery rate. The results show that the extraction rate of four kinds of sulfonamides is the highest when the extraction solvent is about 30% methanol solution and the inorganic salt is two potassium phosphate, the extraction rate of four sulfonamides is the highest. The recovery of a variety of cosmetics and the recovery of SAs The rate range is 81.1~99.5%, and the relative standard deviation RSD is 2.01~4.09%. fifth: the extraction of tetracycline (TCs: tetracycline, oxytetracycline and chlortetracycline) in cosmetics samples with methanol hydrogen phosphate water double aqueous two-phase system, and the rapid determination of tetracycline drugs in cosmetics samples by high performance liquid chromatography (HPLC) technique. The effect of the formation conditions of the biaqueous phase on the extraction rate of tetracycline compounds was investigated. The results showed that when the extraction solvent was about 30% methanol, the methanol was more fully exposed to tetracycline compounds in cosmetics, thus extracting tetracycline like compounds in cosmetics, adding purifier PSA and C_ (18) to adsorb impurities in the upper phase. The objective is to extract three kinds of tetracycline in cosmetics. This method is applied to the extraction and determination of tetracycline compounds in cosmetics. The recovery rate is 87.1~98.1%, and the detection limits are 14.4,18.1 and 19.1 ng/g., respectively.
【学位授予单位】：烟台大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：O657;TQ658

【参考文献】