Study On Chromatography In The Analysis Of Fine Chemicals

Depending on the advantages of high performance liquid chromatography (HPLC) and gas chromatography (GC) in fast separation and accurate quantification, combined with the characteristic of gas chromatography-mass spectrometry (GC-MS) in structure elucidation, the relative substances in some fine chemicals were analyzed for the quality control and technology optimization.The main content of this paper could be expressed as follows:1. The analytical methods were proposed for the determination of para-ester and p-chloroaniline in industrial para-ester by HPLC. Performance was carried out on a C18 column (4.6 mm × 150 mm,5μm), and the chromatographic conditions were optimized by investigating the influences of mobile phase kinds, organic modifier content, pH, and etc, on the retention of the analytes. Three methods were established respectively, including simultaneous determination of para-ester and its related impurities p-chloroaniline by reversed phase ion pair liquid chromatography (RP-IP-HPLC), rapid determination of p-chloroaniline by RP-HPLC, and a method for the further separation of other impurities in para-ester by RP-HPLC which is suitable for the identification of the relative impurities by LC-MS. The established methods are accurate and reliable, which can be used for the quantification of para-ester and p-chloroaniline and qualification of the relative impurities.2. GC and HPLC methods were established for the quantitative analysis of related substances in semifinished condensate liquid of coumarin. Main related substances of coumarin were identified by GC-MS. Furthermore, quantitative analyses of the components including phenol, salicylaldehyde, benzyl acetate, coumarin and disalicylaldehyde were accomplished by GC and HPLC, respectively. GC experiment was carried out on a capillary column (30 m × 0.25 mm × 0.5 μm) and the chromatographic conditions were optimized by adjusting the programmable column temperature gradient. HPLC experiment was carried out on a C18 column (4.6 mm × 150 mm,5 μm), and the chromatographic conditions were optimized by investigating the influences of elution condition of mobile phase on the retention of analytes. The established analytical methods are accurate, rapid and reproducible, which can be used for the simultaneous determination of content of the coumarin and related impurities.