【作者】 高丽荣；

【导师】 杨莉丽；

【作者基本信息】 河北大学 ， 分析化学， 2003， 硕士

【摘要】 论文详细报告了采用氢化物发生-原子荧光光谱法结合预分离、预处理技术对多种中成药、中草药中的不同形态的砷进行了分离分析的应用研究，全文共分五章。 第一章：文献综述。对中药中微量元素的形态分析研究进展情况进行了评述，共引用文献62篇。 第二章：建立了氢化物发生-原子荧光光谱法测定总砷含量的分析方法。考察了仪器的工作条件、酸介质浓度、载流浓度、硼氢化钾浓度和不同增感剂对砷原子荧光强度的影响以及五价砷的还原条件，探讨了多种共存离子对砷测定的干扰和消除方法，在最佳实验条件下，利用所建立的分析方法成功地实现了牛黄清心、牛黄解毒、牛黄上清、银翘解毒等十一种中药丸剂或片剂中总砷含量的分析测定，方法的检出限为90.5ng／L，相对标准偏差为1.38％，样品加标回收率为90.7～108.9％。 第三章：建立了利用氢化物发生-原子荧光光谱法直接测定三价及五价砷的分析方法，对负高压、原子化器温度、原子化器高度、灯电流、载气流量、屏蔽气流量等仪器工作条件、硼氢化钾、还原剂浓度及不同增感剂等实验条件进行了最佳化选择，探讨了共存离子对砷测定的干扰和消除方法，结果表明，方法检出限为89.1ng／L，相对标准偏差为1.24％。利用本方法成功对牛黄清心、黄连解毒两种中药复方中的原生药、残渣、悬浮态及可溶态中的三价及五价砷进行了分析测定，回收率为91.0～109.5％。 第四章：利用离子交换树脂分离技术结合氢化物发生-原子荧光光谱法测定了中草药复方黄连解毒方剂的原生药、残渣、悬浮态及可溶态中的三价及五价砷。对树脂吸附最佳pH、吸附时间、解吸液浓度等树脂静态和动态分离条件进行了最佳化选择，同时考察了仪器的工作条件、试剂浓度、不同增感剂及共存离子等实验条件对荧光强度的影响，结果显示，方法检出限为89.1 ng／L，相对标准偏差为1.42％。利用所建立的两种方法成功地对黄连解毒汤中的三价及五价砷进行了分离测定，回收率介于91.0～109.5％之间。 第五章：建立了树脂动态分离-氢化物发生-原子荧光光谱法测定中成药中三价砷、五价砷和二甲基砷的分离分析方法。对豁酸浸提液浓度和浸提时间、不同解吸液等树脂分离的最佳条件进行了选择，探讨了仪器的」_作条件、试剂浓度、增感剂对砷原子荧光强度的影响。实验结果表明，方法检出限为104.0 ng/L，相对标准偏差为1.41%。利用本方法成功地对/]“)七七珍丹、喉症丸、小儿牛黄散、牛黄解毒丸(片)等多种中成药中的不同形态砷的含量进行了分离分析，回收率为90.8一1 10.2%。更多还原

【Abstract】 The studies of speciation analysis of trace arsenic in Traditional Chinese Medicine by hydride generation-atomic fluorescence spectrometry are reported in this paper, which consists of five chapters.Chapter one: The recent progress on the speciation analysis of trace elements in Traditional Chinese Medicine has been reviewed with the relative references of 62.Chapter two: A method has been described for the determination of arsenic by hydride generation-atomic fluorescence spectrometry (HG-AFS). The experimental conditions that influence the atomic fluorescence intensity and the reduction of arsenic were investigated and optimized, and the influence from foreign ions and the elimination were studied. The detection limit and relative standard deviation (RSD) were of 90.5ng/L and 1.38%, respectively. The proposed method was applied to the determination of arsenic in eleven kinds of Traditional Chinese Medicines produced by different manufactures with a recovery range of 90.7-108.9%.Chapter three: A method has been described for the direct determination of arsenic species (arsenite, arsenate) in Traditional Chinese Medicines using hydride generation-atomic fluorescence spectrometry (HG-AFS). The experimental conditions that influence the fluorescence intensity and the reduction of arsenic were investigated and optimized, and the influence from foreign ions and the elimination were studied. The detection limit of 89.1 ng/L was obtained. The proposed method was applied to the determination of arsenic species in water leachate of Traditional Chinese Medicine with a recovery range of 91.0-109.5%.Chapter four: A method for the determination of arsenic species (arsenite, arsenate) in Traditional Chinese Medicines using hydride generation-atomic fluorescence spectrometry (HG-AFS) with anion exchange resin separation has been studied. The anion exchange resin was used to separate arsenite and arsenate. The separation conditions were investigated and optimized. The experimental conditions that influence the fluorescence intensity and the reduction of arsenic (V) wereinvestigated and optimized, and the influence from foreign ions and the elimination were studied. It was applied to the determination of arsenic species in water leachate of Traditional Chinese Medicines. The detection limit ol 89.1 ng/L and a recovery range of 91. 1-109. 3% were obtained.Chapter five: A method has been described for the determination of arsenic species (arsenite, arsenate and dimethylarinic acid) in Traditional Chinese Patent Medicine by hydride generation-atomic fluorescence spectrometry (HG-AFS) using separation with ion-exchange resin column. The extraction of arsenic with mechanical shaking, the separation of arsenic species with ion-exchange column and the influence of experimental conditions on the fluorescence intensity were investigated and optimized. The detection limit was found to be 104.0 ng/L. The proposed method was successfully applied to the determination of arsenite, arsenate and dimethylarinic acid in Traditional Chinese Patent Medicine with a recovery range of 90.8- 110.2%.更多还原