【摘要】：本論文充分利用高效液相色譜法(HPLC)和氣相色譜法(GC)快速分離、準(zhǔn)確定量的優(yōu)勢,并結(jié)合氣相色譜-質(zhì)譜聯(lián)用(GC-MS)技術(shù)在定性方面的特點,對幾種精細(xì)化工產(chǎn)品中的相關(guān)物質(zhì)進(jìn)行分析研究,所建立的分析方法對于精細(xì)化工產(chǎn)品生產(chǎn)工藝的改進(jìn)和控制具有指導(dǎo)意義,可服務(wù)于精細(xì)化工生產(chǎn)。本文的具體內(nèi)容如下：1.建立了利用HPLC測定工業(yè)對位酯中對位酯及其相關(guān)雜質(zhì)對氯苯胺含量的方法。在C18色譜柱(4.6×150 mm,5 μm)上通過考察流動相種類、有機調(diào)節(jié)劑比例、pH值等對保留的影響來優(yōu)化色譜條件。分別建立了同時測定對位酯和對氯苯胺的反相離子對高效液相色譜法、快速測定對氯苯胺的反相高效液相色譜法,并進(jìn)一步建立了分離對位酯中其他相關(guān)雜質(zhì)的反相高效液相色譜法,可用于對位酯中相關(guān)雜質(zhì)的液相色譜-質(zhì)譜聯(lián)用定性分析。所建立的方法準(zhǔn)確、可靠,可用于對位酯和對氯苯胺的含量測定以及相關(guān)雜質(zhì)的定性,有助于對位酯工業(yè)品的質(zhì)量控制。2.建立了香豆素半成品縮合液中相關(guān)物質(zhì)的氣相色譜和高效液相色譜的分析方法。利用GC-MS對工業(yè)合成香豆素半成品縮合液中的相關(guān)物質(zhì)進(jìn)行定性分析,并分別利用GC和HPLC對主要成分苯酚、水楊醛、乙酸苯酯、香豆素和二聚水楊醛五種物質(zhì)進(jìn)行含量測定。對于氣相色譜法,通過在毛細(xì)管氣相色譜柱(30m×0.25 mm×0.5 μm)上優(yōu)化程序升溫梯度來優(yōu)化色譜條件,對于高效液相色譜法,在C18色譜柱(4.6×150 mm,5 μm)上通過考察流動相種類、有機調(diào)節(jié)劑比例對保留的影響來優(yōu)化色譜條件。所建立的分析方法準(zhǔn)確、快速、重復(fù)性好,可用于同時測定工業(yè)合成香豆素半成品縮合液中相關(guān)物質(zhì)含量,并用于質(zhì)量控制并指導(dǎo)生產(chǎn)工藝改進(jìn)。
[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.
【學(xué)位授予單位】：南京大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2016
【分類號】：O657.7;TQ07

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1 韋蘭春;色譜法在精細(xì)化學(xué)品分析中的應(yīng)用研究[D];南京大學(xué);2016年

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本文編號：2337115