本文選題：化妝品 + 雙水相體系�。� 參考：《煙臺大學(xué)》2017年碩士論文

【摘要】：隨著人們生活水平與健康意識的提高,各類化妝品中可能存在的有機污染物與化學(xué)添加物質(zhì)(如:抗氧化劑、抗生素、抗紫外劑等)的種類與含量引起了消費者的重視,與之相關(guān)的檢測技術(shù)問題也受到研究者的關(guān)注。目前用于各種化合物檢測的儀器已經(jīng)能夠滿足檢測的要求,由于化妝品樣品基體的復(fù)雜性,因此在檢測過程中樣品前處理技術(shù)是制約化合物檢測的主要因素。論文對化妝品中六種苯系物(BTEX)、兩種抗氧化劑(BHA、BHT)、磺胺類藥物和四環(huán)素類藥物的現(xiàn)有的前處理方法及檢測方法進行了綜述,采用雙水相基質(zhì)去除法作為樣品前處理技術(shù)高效提取化妝品中的目標(biāo)物質(zhì),結(jié)合氣相色譜-質(zhì)譜聯(lián)用(GC-MS)和高效液相色譜(HPLC)實現(xiàn)了目標(biāo)物質(zhì)的快速、準(zhǔn)確測定。論文主要分為五個部分:第一部分:闡述化妝品樣品常用的前處理方法,并說明了本文的研究意義和主要研究內(nèi)容。第二部分:基于異丙醇-(NH_4)2SO_4-H_2O雙水相樣品的預(yù)處理的方法,運用氣相色譜-質(zhì)譜聯(lián)用(GC-MS)建立了一種環(huán)境友好型檢測化妝品樣品中六種苯系物(苯、甲苯、乙苯、對二甲苯、間二甲苯和鄰二甲苯)的方法。實驗考察了雙水相的形成條件,并探討了不同含水量的化妝品樣品對雙水相萃取率的影響。結(jié)果顯示,與有機溶劑乙腈和乙醇相比,異丙醇破乳作用最好;異丙醇和水的體積比對化妝品中六種苯系物的提取率有影響,當(dāng)異丙醇與水的體積比大約為2:3時,因為化妝品中的苯系物與異丙醇能夠充分接觸,所以六種苯系物的提取率較高。根據(jù)本方法對化妝品樣品進行測定,回收率為81.1~98.2%,檢出限為1.1~3.9ng/g。第三部分:用異丙醇-NaCl-H_2O雙水相體系基質(zhì)去除法高效提取化妝品樣品中的抗氧化劑(BHA、BHT),結(jié)合氣相色譜-質(zhì)譜聯(lián)用(GC-MS)實現(xiàn)了對化妝品樣品中兩種抗氧化劑的快速準(zhǔn)確測定。實驗考察了有機萃取溶劑、無機鹽、凈化劑及化妝品的含水量對BHA和BHT的萃取影響。結(jié)果表明實驗中選用異丙醇破乳效果最好;體積分?jǐn)?shù)約為40%的異丙醇水溶液為提取液,然后再加入NaCl形成雙水相體系,抗氧化劑進入雙水相上相實現(xiàn)BHA和BHT的高效萃取,此時化妝品中BHA和BHT的萃取效率最高。本方法用于檢測多種市售的化妝品樣品中BHA和BHT,均得到了滿意的結(jié)果。測定回收率為84.1~96.5%,相對標(biāo)準(zhǔn)偏差RSD為2.11~4.03%。步驟簡單、可靠,可很好地應(yīng)用于化妝品中BHA和BHT的快速檢測。第四部分:應(yīng)用雙水相技術(shù)進行樣品預(yù)處理,以HPLC為檢測手段,建立了化妝品中四種磺胺類化合物(SAs:磺胺噻唑(ST),磺胺甲基嘧啶(SM1),磺胺二甲基嘧啶(SM2),磺胺氯噠嗪(SCP))的快速分析方法。配制磺胺類化合物的標(biāo)準(zhǔn)溶液時,實驗發(fā)現(xiàn)用50%的乙腈水溶液作為標(biāo)準(zhǔn)稀釋液時,四種磺胺類藥物峰形最好,回收率最高。實驗考察了雙水相的形成條件及不同含水量的化妝品對磺胺類化合物萃取率的影響,結(jié)果表明,選擇提取溶劑為約30%甲醇水溶液,無機鹽為磷酸氫二鉀時,四種磺胺類藥物的萃取率最高。按照實驗方法對多種化妝品進行檢測,SAs的回收率范圍為81.1~99.5%,相對標(biāo)準(zhǔn)偏差RSD為2.01~4.09%。第五部分:以甲醇-磷酸氫二鉀-水雙水相體系高效提取化妝品樣品中的四環(huán)素類藥物(TCs:四環(huán)素、土霉素和金霉素),結(jié)合高效液相色譜(HPLC)技術(shù)實現(xiàn)了對化妝品樣品中的四環(huán)素類藥物的快速準(zhǔn)確檢測。實驗考察了雙水相的形成條件對四環(huán)素類化合物萃取率的影響,結(jié)果表明,提取溶劑為約30%甲醇時,甲醇與化妝品中的四環(huán)素類化合物接觸更充分,從而萃取化妝品中的四環(huán)素類藥物,上相中加入凈化劑PSA和C_(18)吸附雜質(zhì),目的是高效提取化妝品中的三種四環(huán)素類物質(zhì)。本方法應(yīng)用于化妝品中的四環(huán)素類化合物的提取測定,回收率為87.1~98.1%,檢出限分別為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.
【學(xué)位授予單位】：煙臺大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2017
【分類號】：O657;TQ658

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