【摘要】：染發(fā)劑是較為常見的的美發(fā)產(chǎn)品,氧化型染發(fā)劑具有上色效果好、染色時(shí)間長(zhǎng)和色調(diào)范圍廣等優(yōu)點(diǎn)。染料的主要成分多為苯胺類化合物,具有一定程度的致畸性、致敏性和致癌性,長(zhǎng)期和高頻率使用容易對(duì)人體造成慢性傷害。鑒于國(guó)內(nèi)外研究者越來(lái)越重視人體健康問題,所以加強(qiáng)和完善染發(fā)劑的檢測(cè)技術(shù)勢(shì)在必行。文獻(xiàn)報(bào)道的染料檢測(cè)方法主要有薄層色譜法、毛細(xì)管電泳法、高效液相色譜法、離子色譜法、氣相色譜法、伏安法、氣相色譜-質(zhì)譜法、高效液相色譜-質(zhì)譜法,但單個(gè)系統(tǒng)檢測(cè)的染料種類基本停留在幾種到十幾種,不能較好的滿足染發(fā)劑的日常監(jiān)管。本論文選取了國(guó)家食品藥品監(jiān)督管理總局發(fā)布的32種禁限用染料成分和市場(chǎng)上仍存在檢測(cè)空白的染料為研究對(duì)象,分別建立了相應(yīng)的高效液相色譜-質(zhì)譜法和氣相色譜-質(zhì)譜法測(cè)定氧化型染發(fā)劑中多種禁限用染料,方法操作簡(jiǎn)便、耐用性好、專屬性強(qiáng)。HPLC-MS/MS法和GC-MS/MS法能較好的形成染料檢測(cè)種類的互補(bǔ),可用于染發(fā)劑中染料含量的測(cè)定。主要內(nèi)容如下:1、高效液相色譜-質(zhì)譜法(HPLC-MS/MS)測(cè)定染發(fā)劑中33種禁限用染料。染發(fā)劑樣品用甲醇-抗壞血酸水溶液溶解,用正己烷凈化,以5mmol/L的乙酸銨和乙腈為流動(dòng)相進(jìn)行梯度洗脫,經(jīng)Agilent ZORBAX Extend C18柱(2.1mm*100mm,1.8μm)分離,采用多重反應(yīng)監(jiān)測(cè)模式(MRM)進(jìn)行定性和定量分析。33種染料組分在相應(yīng)的質(zhì)量濃度范圍內(nèi)線性關(guān)系良好,線性相關(guān)系數(shù)(R2)均大于0.99,檢出限為0.01-29.5mg/kg,回收率為71.4%-115.1%,混合標(biāo)準(zhǔn)溶液在32h內(nèi)的穩(wěn)定性的相對(duì)標(biāo)準(zhǔn)偏差小于10%。2、氣相色譜-質(zhì)譜法(GC-MS/MS)測(cè)定染發(fā)劑中40種禁限用染料。染發(fā)劑樣品用甲醇-抗壞血酸水溶液溶解,用正己烷凈化,程序升溫,在Agilent VF-624ms柱(0.25mm*30m,1.4μm)分離,采用多重反應(yīng)監(jiān)測(cè)模式(MRM)進(jìn)行定性和定量分析。40種染料組分在相應(yīng)的質(zhì)量濃度范圍內(nèi)線性關(guān)系良好,線性相關(guān)系數(shù)(R2)均大于0.99,檢出限為4.4-10.7mg/kg,回收率為71.5%-118.6%。實(shí)驗(yàn)分別采用高效液相色譜法、高效液相色譜-質(zhì)譜法和氣相色譜-質(zhì)譜法測(cè)定氧化型染發(fā)劑,樣品數(shù)據(jù)相對(duì)標(biāo)準(zhǔn)偏差基本在5%以內(nèi)。
[Abstract]:Hair dyeing agent is a common hairdressing product. Oxidized hair dye has the advantages of good coloring effect, long dyeing time and wide color range. The main components of dyes are aniline compounds, which are teratogenic, sensitized and carcinogenic to a certain extent. The long-term and high-frequency use of aniline is easy to cause chronic injury to human body. Since researchers at home and abroad pay more and more attention to human health problems, it is imperative to strengthen and improve the detection technology of hair dye. TLC, capillary electrophoresis, high performance liquid chromatography, ion chromatography, gas chromatography, voltammetry, gas chromatography-mass spectrometry, high performance liquid chromatography-mass spectrometry, However, the types of dyes detected by a single system basically stay at a few to more than a dozen, which can not satisfy the daily supervision of hair dyes. In this paper, 32 kinds of banned dyes published by the State Administration of Food and Drug Administration and the dyes that still exist in the market are selected as the research objects. High performance liquid chromatography-mass spectrometry (HPLC-MS) and gas chromatography-mass spectrometry (GC-MS) have been established for the determination of several kinds of forbidden dyes in oxidized hair dyes. The method is easy to operate and has good durability. Strong specificity. HPLC-MS / MS method and GC-MS/MS method can be used for the determination of dye content in hair dye. The main contents are as follows: high performance liquid chromatography-mass spectrometry (HPLC-MS/MS) for the determination of 33 prohibited dyes in hair dyes. The hair dye sample was dissolved in methanol-ascorbic acid aqueous solution, purified by n-hexane, gradient eluted with ammonium acetate and acetonitrile of 5mmol/L as mobile phase, and separated by Agilent ZORBAX Extend C18 column (2.1 mm ~ 100 mm ~ 1.8 渭 m). The qualitative and quantitative analysis of .33 dye components by multiplex reaction monitoring model (MRM) has a good linear relationship within the corresponding mass concentration range. The linear correlation coefficient (R2) is greater than 0.99, the detection limit is 0.01-29.5mg / kg, the recovery is 71.4-115.1. The relative standard deviation of stability of mixed standard solution within 32 hours is less than 100.2.Gas chromatography-mass spectrometry (GC-MS/MS) is used to determine 40 forbidden dyes in hair dye. The hair dye sample was dissolved in methanol-ascorbic acid aqueous solution, purified by n-hexane, programmed with temperature, and separated on Agilent VF-624ms column (0.25mm ~ 30mg ~ (1.4 渭 m). The qualitative and quantitative analysis of 40 dye components with multiple reaction monitoring model (MRM) showed a good linear relationship within the corresponding range of mass concentration. The linear correlation coefficient (R2) was greater than 0.99, the detection limit was 4.4-10.7 mg / kg, and the recovery rate was 71.5 -118.6 mg / kg. High performance liquid chromatography (HPLC), high performance liquid chromatography-mass spectrometry (HPLC-MS) and gas chromatography-mass spectrometry (GC-MS) were used to determine the oxidized hair dye respectively. The relative standard deviation of sample data was less than 5%.
【學(xué)位授予單位】：浙江工業(yè)大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2016
【分類號(hào)】：O657.63;TQ658.34

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