摘要
采用超临界CO2流体色谱技术,同时分析五种禁用偶氮型致敏性分散染料。色谱柱为Shimadzu Wonda Cract ODS-2 C18色谱柱(4.6 mm×250 mm×5μm),紫外检测波长为450 nm,流动相采用夹带极性改性剂甲醇、乙醇和乙腈的超临界态CO2流体。以容量因子、分离度和选择性为指标,考察了改性剂及其配比、背压、流速和柱温对分离效果的影响。在甲醇、乙醇和乙腈三种改性剂中,甲醇为最好的改性剂。在体积分数10%甲醇作为改性剂时,各分子间的分离度均可达到1.5以上。以10%甲醇为改性剂,考察了柱温、柱压和流速对五种偶氮型致敏性分散染料分离效果的影响。优化后的分离条件为:改性剂10%甲醇,流速1.20 m L/min,柱温36℃,背压10 MPa。在此色谱条件下,五种偶氮型致敏性分散染料能够达到基线分离,分离时间约为12 min。
The simultaneous analysis of five banned azo-type allergenous disperse dyes is carried out by supercritical fluid chromatography in this research. Shimadzu Wonda Cract ODS-2 C18 column （4.6 mm× 250 mm×5 μm） is used as the separation column, UV detection wavelength is 450 nm, and supercritical CO2 fluid with methanol, ethanol and acetonitrile is used as mobile phase. The influence of type and con- centration of alcohol modifier, back pressure, flow rate and column temperature on retention factor, dia- stereoselectivity and resolution is studied. Among methanol, ethanol and acetonitrile, methanol turns out to be the most favorable modifier, and 10% （V/V） of methanol is chosen as the suitable concentra- tion at which every allergenous disperse dye could be separated with resolution≥1.5. The effects of back pressure, flow rate and column temperature are investigated at 10% （V/V） of methanol in the pres- sure range of 10N20 MPa, flow rate from 1.00 mL/min to 2.00 mL/min and temperature range from 30 ℃ to 45 ℃. Under the optimum separation conditions of 10% （V/V） of methanol modifier as mobile phase, 1.20 mL/min of flow rate for mobile phase, 36 ℃ of column temperature and 10 MPa of back pressure, the five banned azo-type allergenous disperse dyes could be separated completely and the running time is about 12min.
出处
《印染》
北大核心
2016年第20期38-42,共5页
China Dyeing and Finishing
