色谱法在精细化学品分析中的应用研究
发布时间：2018-11-17 08:21
【摘要】：本论文充分利用高效液相色谱法(HPLC)和气相色谱法(GC)快速分离、准确定量的优势,并结合气相色谱-质谱联用(GC-MS)技术在定性方面的特点,对几种精细化工产品中的相关物质进行分析研究,所建立的分析方法对于精细化工产品生产工艺的改进和控制具有指导意义,可服务于精细化工生产。本文的具体内容如下：1.建立了利用HPLC测定工业对位酯中对位酯及其相关杂质对氯苯胺含量的方法。在C18色谱柱(4.6×150 mm,5 μm)上通过考察流动相种类、有机调节剂比例、pH值等对保留的影响来优化色谱条件。分别建立了同时测定对位酯和对氯苯胺的反相离子对高效液相色谱法、快速测定对氯苯胺的反相高效液相色谱法,并进一步建立了分离对位酯中其他相关杂质的反相高效液相色谱法,可用于对位酯中相关杂质的液相色谱-质谱联用定性分析。所建立的方法准确、可靠,可用于对位酯和对氯苯胺的含量测定以及相关杂质的定性,有助于对位酯工业品的质量控制。2.建立了香豆素半成品缩合液中相关物质的气相色谱和高效液相色谱的分析方法。利用GC-MS对工业合成香豆素半成品缩合液中的相关物质进行定性分析,并分别利用GC和HPLC对主要成分苯酚、水杨醛、乙酸苯酯、香豆素和二聚水杨醛五种物质进行含量测定。对于气相色谱法,通过在毛细管气相色谱柱(30m×0.25 mm×0.5 μm)上优化程序升温梯度来优化色谱条件,对于高效液相色谱法,在C18色谱柱(4.6×150 mm,5 μm)上通过考察流动相种类、有机调节剂比例对保留的影响来优化色谱条件。所建立的分析方法准确、快速、重复性好,可用于同时测定工业合成香豆素半成品缩合液中相关物质含量,并用于质量控制并指导生产工艺改进。
[Abstract]:In this paper, the advantages of rapid separation and quantification of (HPLC) and (GC) by high performance liquid chromatography (HPLC) and gas chromatography (GC) were fully utilized, and combined with the qualitative characteristics of GC-MS (gas chromatography-mass spectrometry). The related substances in several kinds of fine chemical products are analyzed and studied. The analytical method established in this paper is of guiding significance for the improvement and control of fine chemical production process and can serve the fine chemical production. The specific contents of this paper are as follows: 1. A method for the determination of p-chloroaniline and its related impurities in industrial para-esters by HPLC was established. The chromatographic conditions were optimized on C18 column (4.6 脳 150 mm,5 渭 m) by investigating the effects of mobile phase, organic modifier ratio and pH value on retention. A reversed phase ion-pair high performance liquid chromatography (RP-HPLC) for the simultaneous determination of para-chloroaniline and p-chloroaniline was established, and a rapid RP-HPLC method for the determination of p-chloroaniline was developed. A RP-HPLC method for the separation of other related impurities in para-ester was established, which can be used for qualitative analysis of related impurities in para-ester by liquid chromatography-mass spectrometry (LC-MS). The established method is accurate and reliable. It can be used for the determination of p-chloroaniline and para-chloroaniline and the qualitative determination of related impurities, which is helpful to the quality control of para-ester industrial products. 2. A method for the determination of related substances in coumarin semi-finished product condensation solution by gas chromatography and high performance liquid chromatography was established. The related substances in the condensation solution of industrial synthesis coumarin semi-finished product were qualitatively analyzed by GC-MS. The contents of phenol, salicylaldehyde, benzyl acetate, coumarin and salicylidene dimer were determined by GC and HPLC, respectively. For gas chromatography, the temperature gradient was optimized on a capillary gas column (30 m 脳 0.25 mm 脳 0. 5 渭 m), and for high performance liquid chromatography (HPLC) on a C18 column (4. 6 脳 150 mm,). At 5 渭 m, the chromatographic conditions were optimized by investigating the influence of the mobile phase and the proportion of organic modifier on the retention. The established analytical method is accurate, rapid and reproducible. It can be used to simultaneously determine the content of related substances in the condensation solution of industrial synthetic coumarin semi-finished products, and to control the quality and guide the improvement of production process.
【学位授予单位】：南京大学
【学位级别】：硕士
【学位授予年份】：2016
【分类号】：O657.7;TQ07
本文编号：2337115
[Abstract]:In this paper, the advantages of rapid separation and quantification of (HPLC) and (GC) by high performance liquid chromatography (HPLC) and gas chromatography (GC) were fully utilized, and combined with the qualitative characteristics of GC-MS (gas chromatography-mass spectrometry). The related substances in several kinds of fine chemical products are analyzed and studied. The analytical method established in this paper is of guiding significance for the improvement and control of fine chemical production process and can serve the fine chemical production. The specific contents of this paper are as follows: 1. A method for the determination of p-chloroaniline and its related impurities in industrial para-esters by HPLC was established. The chromatographic conditions were optimized on C18 column (4.6 脳 150 mm,5 渭 m) by investigating the effects of mobile phase, organic modifier ratio and pH value on retention. A reversed phase ion-pair high performance liquid chromatography (RP-HPLC) for the simultaneous determination of para-chloroaniline and p-chloroaniline was established, and a rapid RP-HPLC method for the determination of p-chloroaniline was developed. A RP-HPLC method for the separation of other related impurities in para-ester was established, which can be used for qualitative analysis of related impurities in para-ester by liquid chromatography-mass spectrometry (LC-MS). The established method is accurate and reliable. It can be used for the determination of p-chloroaniline and para-chloroaniline and the qualitative determination of related impurities, which is helpful to the quality control of para-ester industrial products. 2. A method for the determination of related substances in coumarin semi-finished product condensation solution by gas chromatography and high performance liquid chromatography was established. The related substances in the condensation solution of industrial synthesis coumarin semi-finished product were qualitatively analyzed by GC-MS. The contents of phenol, salicylaldehyde, benzyl acetate, coumarin and salicylidene dimer were determined by GC and HPLC, respectively. For gas chromatography, the temperature gradient was optimized on a capillary gas column (30 m 脳 0.25 mm 脳 0. 5 渭 m), and for high performance liquid chromatography (HPLC) on a C18 column (4. 6 脳 150 mm,). At 5 渭 m, the chromatographic conditions were optimized by investigating the influence of the mobile phase and the proportion of organic modifier on the retention. The established analytical method is accurate, rapid and reproducible. It can be used to simultaneously determine the content of related substances in the condensation solution of industrial synthetic coumarin semi-finished products, and to control the quality and guide the improvement of production process.
【学位授予单位】：南京大学
【学位级别】：硕士
【学位授予年份】：2016
【分类号】：O657.7;TQ07
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1 韦兰春;色谱法在精细化学品分析中的应用研究[D];南京大学;2016年
，本文编号：2337115
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