【作者】 宋书娟；

【导师】 宋启军；

【作者基本信息】 江南大学 ， 分析化学， 2007， 硕士

【摘要】 海因类物质是一种高效、安全杀菌消毒剂,具有强烈杀灭真菌、细菌及病毒的效果。其稳定性好、反应活性高,广泛应用于医药、化工和农业等行业。三氯生是一种广谱抗菌剂和防腐剂,广泛应用于个人护理产品并且也适用于作为聚合物和纤维的添加剂使这些材料具有抗菌性能。本论文主要对海因类和三氯生消毒剂物质的化学发光体系进行了研究,并建立了检测二溴海因、三氯生消毒剂的化学发光测定方法,并探讨了这两种体系的发光机理。主要研究内容如下:1.在鲁米诺-二溴海因（DBDMH）体系中,研究了各因素对体系的影响,确定了最佳反应条件。二溴海因在1.0×10^-10mol·dm^-3～3.0×10-6mol·dm^-3范围内呈良好线性关系,该法检测限为6.2×10-11mol·dm^-3。同时该方法对其它常见离子也有相当的允许量,对二溴海因的选择性良好。2.运用流动注射化学发光法研究了海因类消毒剂的稳定性,包括二溴海因、溴氯海因以及二氯海因。选用的发光试剂为pH值12.2、摩尔浓度1.0×10^-5mol·dm^-3鲁米诺溶液,缓冲体系为0.15mol·dm^-3的三羟甲基氨基甲烷（Tris）溶液。针对不同温度下、不同加入量的丙酮、加入干扰离子以及不同pH值下海因类消毒剂的稳定性进行了详细探讨。并运用毛细管电泳法分离海因类消毒剂中具有氧化性的活性成分,在进样时间为5s、进样高压10kV、分离电压为15kV、pH值为5.8的10mmol·dm^-3的磷酸二氢钾-磷酸氢二钠缓冲体系中实现明显分离,并对可能的活性组分进行了讨论。3.发现了N-溴代琥珀酰亚胺（NBS）-三氯生（TCS）光照-化学发光现象,考察几种常用的氧化剂与光照后的三氯生的化学发光的反应,建立了NBS- TCS体系的化学发光检测方法。优化该体系的反应条件,三氯生浓度在3.5×10-7 1.7×10-4mol·dm^-3范围内与发光强度呈良好的线性关系,检测限为1.0×10-7mol.dm^-3。并进行该体系的离子干扰研究,然后将其应用于实际牙膏样品的检测分析。4.建立三氯生的在线检测方法,包括光照在内在6分钟内可以实现检测,检测限为5.0×10-8mol·dm^-3。该方法对其它常见离子也有相当的允许量。考察不同因素对反应体系的影响,并对其发光机理进行初步探讨。更多还原

【Abstract】 Halogenated dimethylhydantoin derivatives, including 1,3-dibromo-5,5- dimethylhy -dantoin （DBDMH）,1-bromo-3-chloro-5,5-dimethyl-hydantoin（BCDMH）and1,3-dichloro-5,5-dimethylh- -ydantoin （DCDMH）, are specially effective in disinfection of various fungus,bacteria,virus and therefore they are widely used as disinfectants in water treatment as well as in many other area. Triclosan is a broad-spectrum antibacterial and preservative agent which is widely used in personal care products and it is also suitable for incorporation in polymers and fibers to give these materials antibacterial properties. This paper studied the chemiluminecence system of halogenated dimethylhydantoin and triclosan. And these methods were developed for the determination of these substances. The mechanisms were also discussed. The main results were given as follows:1. In the system of Luminol-DBDMH, several factors were studied and the optimal conditions were obtained. The CL intensities were linear with DBDMH concentrations in the range of 1.0×10^-10 mol·dm^-3～3.0×10-6mol·dm^-3. The detection limit of the method was 6.2×10-11mol·dm^-3. Most of the foreign substances tested showed relatively high tolerance levels and the proposed method was successfully applied to the determination of DBDMH in real samples.2. The stability of these compounds in aqueous solution was investigated by using flow injection chemiluminescence （FIA-CL） method. The determination procedure was optimized and the optimum conditions were found to be: pH12.2, 1.0×10^-5mol·dm^-3 of luminol solution, 0.15 mol·dm^-3 of Tris buffer. At the optimized conditions the effects of temperature, pHs, addition of acetone and various interference substances on the stability were investigated in details. Capillary electrophoresis separation of active ingredients in hydantoin derivatives were achieved. Samples were introduced to the capillary by electrokinetic injection by applying a 10 kV for 5 s. After completion of sample injection, 15 kV was applied for 15 min. A solution containing 10 mmol·L-1 potassium dihydrogen phosphate （pH5.8） was used as the running buffer.3. It was found that NBS-TCS system have photo-chemiluminescence phenomenon. Several oxidants react with TCS irradiated with visible light were compared. NBS-TCS system was developed for the determination of TCS. At the optimized conditions, The CL intensities were linear with TCS concentrations in the range of 3.5×10-7 1.7×10-4mol·dm^-3. The detection limit was 1.0×10-7mol·dm^-3. Most of the foreign substances tested showed relatively high tolerance levels and the proposed method was successfully applied to the determination of TCS in toothpaste samples.4. An on-line flow injection chemiluminescence method for the determination of triclosan was proposed. The whole process of analysis, including the online phototransformation and subsequent chemiluminescence detection could be completed in 6 minutes. The detection limit was 5.0×10-8mol·dm^-3. Most of the foreign substances tested showed relatively high tolerance levels. Several factors that influence the Photo-CL reaction and the possible mechanism of the system were discussed.更多还原