【作者】 龚雪云；

【导师】 石杰；

【作者基本信息】 郑州大学 ， 分析化学， 2004， 硕士

【摘要】 原子荧光光谱法是基于原子发射光谱法和原子吸收光谱法的光谱分析技术。作为一种独特的痕量分析技术，原子荧光光谱法具有灵敏度高，选择性好，快速，简便等特点，近年来在痕量分析领域得到了广泛应用。 随着中药事业的不断发展，中药及其制剂在世界范围内防病、治病作用被重新认识，并日益受到重视。中药中的微量元素进入人体后，对人体健康起到重要作用。由于种植环境和条件的影响，这些药材中往往含重金属元素。这些元素的摄入量与人体的健康有密切关系，如汞、铅、砷等元素，在正常的情况下，人体可能耐受的剂量极小，剂量稍高，就可能出现毒副作用。许多国家对进口药材中重金属元素含量作了严格控制，中国作为中药材资源丰富和使用广泛的国家，对中药中重金属元素含量进行分析研究，制定统一、方便、有效的分析测定标准及方法，保证药品质量和用药安全已迫在眉睫。 吸烟有害人体健康，已成为人们普遍重视的社会和医学问题。世界各国都在积极开展低毒、安全香烟的研究。因此，对烟叶中重金属元素的含量进行分析、测试是非常必要的。 食物是人体内的重金属元素的一个重要来源，世界卫生组织和我国卫生部门都对食品中的重金属元素含量制订了限量标准。对粮食中重金属元素含量进行测试具有重要意义。 本论文主要在原子荧光光谱法应用于中药、烟草和粮食中的汞、铅、锑等元素的测定方面作了以下工作： 1．采用HNO₃-H₂O₂的湿法消解体系，研究了冷原子荧光法用于粮食中汞含量的测定。同时，比较了三种不同的湿法消解体系，讨论了氯化严锡浓度、负高压、载气流量、还原时间等的影响。对样品的前处理方法和仪器工作条件进行了探讨和优化。在选定的实验条件下，工作曲线在0—4.0ug/L的浓度范围内线性良好，相关系数为0.9999，检出限为0.03ug/L，回收率为91％～108％，测定了原阳大米和中牟麦仁中的汞含量，得到了满意的结果。 2．应用AFS—2202a型双道原子荧光分光光度计，采用高压溶样的消解方式，在选定的实验条件下，建立了氢化物发生—原子荧光光谱法测定烟叶中汞含量的方法。同时，研究了光电管负高压，灯电流，原子化器高度，载气和屏蔽气郑州人学倾}_学位论交流量，硼氢化钾浓度等因素对测定结果的彩l响。在选定实验条卞日‘，卜作曲线在0一8、Jg/IJ的浓度范围线性良好，相关系数为0.(，999，求的检出限为（）.（）2魄/l.，加标回收率为90%一105%，相对标准偏差为1.3%。以工作曲线法测定了瓦利，不同产地的烟仆卜样品中的汞含量。 3.应川Al:S一22O2a型双道原子荧光分光光度计和断续流动的氛化物发’{几技术，采用高压溶样的消解方式，在选定的实验条件下，建立了氢化物发生一原子荧光光谱法测定中药和烟仆}。中铅含量的方法。研究了仪器条件（负高压、幻一电流、原子化器高度、载气.流量、屏蔽气流量、读数时间、延迟时间等）对测定结果的影响，同时对硼氢化钾浓度，载流，氧化体系，酸度，」二扰离子等囚索进行了探讨。在选定实验条件下，工作曲线在O一400ug/LJ浓度范}_l}l内线性良好，相关系数为0.9998，铅的检出限为0.18瑰/L，加标回收率为91%一109%，相刘‘标准偏差为1.2%。以工作曲线法测定了十种中药样品、五种不同产地的烟叶样品和一十一种不同产地、不同炮制方法的牛膝中的错含量。 4.应川川‘S一2202a型双道原子荧光分光光度计和断续流动的氢化物发生技术，采用高压溶样的消解方式，在选定的实验条件下，建立了氢化物发生一原子荧光光潜法测定中药和烟叶中锑含量的方法。研究了仪器条件（负高压、灯电流、原子化器高度、载气流量、屏蔽气流量、读数时问、延迟时间等）对测定结果的影响，卜小时对硼氢化钾浓度，还原剂，酸度，}几扰离J二等因索进行了探讨。在选定实验条州下，工作曲线在O一拍[」g/l」浓度范困内线性良好，相关系数为0.9999，锑的检出限为0.14林g/L，加标回收率为93%一107%，相对标准偏差为1.5%。以工作曲线法测定了九种中药样粼:、₁11种不同产地的烟叶样.异，和十·种不同产地、不同炮制方法的牛膝中的锑含最。更多还原

【Abstract】 Atomic fluorescene Spectrometry(AFS) is analysis technology between atomic absorption spectrometry and atomic emission spectrometry. As an special analysis way, AFS possess extending good advantages such as high sensitivity, selectivity, convinence and accuracy, then it is widely used in trace-elemental analysis fields in recent years.With the continous and exciting development of Chinese Traditional Medicine, it is well known that Chinese Traditional Medicine play a great role in the prevention and cure of some disease and make a strong impact on our health. However, owing to the influence of the planting conditions, there are such poisionous elements such as mercury,lead in Chinese Traditional Medicine. Then the contents of some poisionous elements in Chinese Traditional Medicine should be controlled rigidly and it is crucial for our country to establish some simple, united, fast and valid analytical method, so we can keep the drugs’ trait and take medicines safely.This paper is focused on the determination of trace mercury, lead and antimony. The atomic fluorescence spectrometry was used in measuring these elements in Chinese Traditional Medicine, tobacco and grain. As Col lowing: 1. The determination of trace mercury in grain was studied by CVAFS. The pretreatrnent ways of sample and the experimental conditions have been optimized respectively.Good linearity was observed over 0-4. 0ug/L with a detection limi t of 0. 03ug/L and a correlation coefficient of 0. 9999. The recovery was from 91% to 108%.Trace mercury in the standard reference substance was also determined according to this way and the result was in good agreement with recommended value. We also studied the mercury contents in grain by the working curve method. It proves to be simple, rapid, sensitive and convinent.2. A hydride generation atomic fluorescence spectroniotry method has been developed for the determination of trace mercury in tobacco.A high-pressure digestion way using HN03-H202 system was applied for the pretreatment of samples and the interval flow precedure was used. The experimental conditions and instrumental operation parameters such as KBH4 concentration, flow rate of the carrier and shield gas, currents of lamp and height of atomic oven which affect the determination had been optimized respectively. There was a good linear relationship between the fluorescence intensity and mercury concentration in the range of 0-8ug/l with a correlation coefficient of 0.9999,while detection limit was 0. 02ug/L, and the recovery from 90% to 105%. The coefficient of variation was 1.3%. We studied the mercury contents in five kinds of different producing area tobacco.3. A hydride generation atomic fluorescence spectrometry method has been developed for the determination of trace lead in Chinese Traditional Medicine and tobacco. A high-pressure digestion way using HNO4-H2O2 system was applied for the pretreatment of samples and the interval flow precedure was used.The experimental conditions and instrumental operation parameters such as KBH4 concentration, flow rate of the carrier and shield gas, currents of lamp and height of atomic oven which affect, the determination had been optimized respectively. There was a good 1 (near relationship between the fluorescence intensity and lead concentration in the range of 0-400ug/L with a correlation coefficient of 0. 999K, while detection limit was 0. 18ug/L, and the recovery from 91% to 109%. The coefficient of variation was 1.2%. We studied the lead contents in ten kinds of Chinese Traditional Medicine, eleven kinds of different producing area niuxi and five kinds of different producing area tobacco.4. A hydride generation atomic fluorescence spectrometry method has been developed for the determination of trace antimony in ChineseTraditional Medicine and tobacco. A high-pressure digestion way using I1N03~H202 system was applied for the pretreatrnent of samples and the interval flow procedure was used. The experimental conditions and instrumental operation parameters such as KBI14 concentration更多还原