高效液相色谱—质谱法和气相色谱—质谱法测定染发剂中多种禁限用染料
发布时间：2018-09-19 12:56
【摘要】：染发剂是较为常见的的美发产品,氧化型染发剂具有上色效果好、染色时间长和色调范围广等优点。染料的主要成分多为苯胺类化合物,具有一定程度的致畸性、致敏性和致癌性,长期和高频率使用容易对人体造成慢性伤害。鉴于国内外研究者越来越重视人体健康问题,所以加强和完善染发剂的检测技术势在必行。文献报道的染料检测方法主要有薄层色谱法、毛细管电泳法、高效液相色谱法、离子色谱法、气相色谱法、伏安法、气相色谱-质谱法、高效液相色谱-质谱法,但单个系统检测的染料种类基本停留在几种到十几种,不能较好的满足染发剂的日常监管。本论文选取了国家食品药品监督管理总局发布的32种禁限用染料成分和市场上仍存在检测空白的染料为研究对象,分别建立了相应的高效液相色谱-质谱法和气相色谱-质谱法测定氧化型染发剂中多种禁限用染料,方法操作简便、耐用性好、专属性强。HPLC-MS/MS法和GC-MS/MS法能较好的形成染料检测种类的互补,可用于染发剂中染料含量的测定。主要内容如下:1、高效液相色谱-质谱法(HPLC-MS/MS)测定染发剂中33种禁限用染料。染发剂样品用甲醇-抗坏血酸水溶液溶解,用正己烷净化,以5mmol/L的乙酸铵和乙腈为流动相进行梯度洗脱,经Agilent ZORBAX Extend C18柱(2.1mm*100mm,1.8μm)分离,采用多重反应监测模式(MRM)进行定性和定量分析。33种染料组分在相应的质量浓度范围内线性关系良好,线性相关系数(R2)均大于0.99,检出限为0.01-29.5mg/kg,回收率为71.4%-115.1%,混合标准溶液在32h内的稳定性的相对标准偏差小于10%。2、气相色谱-质谱法(GC-MS/MS)测定染发剂中40种禁限用染料。染发剂样品用甲醇-抗坏血酸水溶液溶解,用正己烷净化,程序升温,在Agilent VF-624ms柱(0.25mm*30m,1.4μm)分离,采用多重反应监测模式(MRM)进行定性和定量分析。40种染料组分在相应的质量浓度范围内线性关系良好,线性相关系数(R2)均大于0.99,检出限为4.4-10.7mg/kg,回收率为71.5%-118.6%。实验分别采用高效液相色谱法、高效液相色谱-质谱法和气相色谱-质谱法测定氧化型染发剂,样品数据相对标准偏差基本在5%以内。
[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%.
【学位授予单位】：浙江工业大学
【学位级别】：硕士
【学位授予年份】：2016
【分类号】：O657.63;TQ658.34
本文编号：2250187
[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%.
【学位授予单位】：浙江工业大学
【学位级别】：硕士
【学位授予年份】：2016
【分类号】：O657.63;TQ658.34
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