中药中不同形态汞、砷和锑的原子荧光光谱分析研究
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摘要
论文详细介绍了采用原子荧光光谱法结合预分离、预处理技术对多种中成药、中草药中不同形态的汞、砷和锑进行分离分析的应用研究。全文共分为6章。
第1章：文献综述。对氢化物发生-双道原子荧光光谱法的应用和中药中微量元素的形态分析研究进展进行了评述。共引用文献88篇。
第2章：建立了蒸气发生-原子荧光光谱法测定总汞含量的分析方法。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汞原子荧光强度的影响；提出用硫脲—柠檬酸—Fe~(3+)作为增感剂增强汞的荧光信号；探讨了共存离子对汞测定的干扰和消除方法。在最佳实验条件下，将本法成功应用于人参再造丸等6种中药样品中总汞含量的分析测定，方法的检出限为5.748μg／L，相对标准偏差为1.56％，回收率为90.4％～109.6％。
第3章：建立了蒸气发生-原子荧光光谱法测定中草药复方方剂原生药、残渣、悬浮态、可溶态无机汞和有机汞的方法。研究了仪器的工作条件、试剂浓度、增感剂对汞原子荧光强度的影响及有机汞的氧化条件，探讨了共存离子对汞测定的干扰和消除方法，利用本方法成功地对万氏牛黄清心方剂中的汞进行了形态分析。方法检出限为7.611 ng／L，RSD为1.24％，回收率为90.3％-110.3％。
第4章：建立了一种氢化物发生-双道原子荧光光谱法同时测定中药中As(Ⅲ)、As(Ⅴ)、Sb(Ⅲ)和Sb(Ⅴ)的方法。研究了仪器的工作条件、试剂浓度对砷和锑原子荧光强度的影响以及五价砷、五价锑的还原条件，探讨了共存离子对砷和锑测定的干扰和消除方法。在最佳工作条件下，砷和锑的最低检出限分别为90.31ng／L和57.82ng／L，相对标准偏差分别为2.01％和1.39％。将本法成功应用于板蓝根颗粒等7种中药样品中砷和锑的形态分析，As(Ⅲ)和As(Ⅴ)的回收率分别为90.1％～105.0％和89.2％～102.0％，Sb(Ⅲ)和Sb(Ⅴ)的回收率分别为89.7％～102.0％和90.3％～110.0％。
第5章：建立了巯基棉分离吸附-氢化物发生-原子荧光光谱法测定中药中As(Ⅲ)和As(Ⅴ)的方法。在1mol／L盐酸介质中，巯基棉定量吸附As(Ⅲ)，不吸附As(Ⅴ)，
摘要
实现了As(III)和As(v)的分离。研究了仪器的工作条件、试剂浓度及不同增感剂对
砷原子吸收信号强度的影响和砷(V)的还原条件，探讨了共存离子对砷测定的干扰
和消除方法，利用本方法成功地对牛黄清火丸等5种中成药中的砷进行了形态分
析。方法检出限为64.3 ing几，RsD为1.120，0，回收率为90.2%一116.30，0。
第6章:建立了一种蒸气发生一双道原子荧光光谱法同时测定中药中汞和砷的
方法，考察并优化了影响荧光强度的实验条件;提出用硫脉一柠檬酸一Fe3+作为增感
剂增强汞和砷的荧光信号;探讨了共存离子对汞和砷测定的干扰及消除方法。在
最佳工作条件下，汞和砷的最低检出限分别为21 .10ng/L和103.Ing/L，相对标准
偏差分别为2.01%和2.39%。将本法成功应用于牛黄清胃丸等6种中药样品中汞和
砷的测定，汞和砷的回收率分别为90.7%一1 10.6%和91.2%一108.5%。
The studies of speciation analysis of mercury, arsenic and antimony in Traditional Chinese Medicine by atomic fluorescence spectrometry are described in this disertation, which consists of six chapters.
Chapter one: The recent progress of the application of hydride generation-double channel atomic fluorescence spectrometry and the speciation analysis of elements in Traditional Chinese Medicine has been reviewed with the relative references of 88.
Chapter two: A method has been described for the determination of mercury by vapor generation-atomic fluorescence spectrometry. The experimental conditions that influence the atomic fluorescence signal intensity were investigated and optimized, and the influence from foreign ions and the elimination were studied. Thiourea-citric acid-ferrite ion was selected as enhancement reagent. The detection limit and relative standard deviation were of 5.748jj,g/L and 1.56 %, respectively. The proposed method was applied to the determination of mercury in six kinds of Traditional Chinese Medicines with a recovery range of 90.4-109.6%.
Chapter three: A sensitive method has been proposed for the determination of inorganic mercury and total organic mercury in Traditional Chinese Medicine by vapor generation-atomic fluorescence spectrometry. The experimental conditions that influence the atomic fluorescence signal intensity of Hg and the oxidization of organic mercury were investigated and optimized. Thiourea-citric acid was selected as sensitization reagent. The influence from foreign ions and their elimination were studied. The detection limit of the method for Hg was of 7.611 ng/L and the relative standard deviation was 1.24%. The proposed method was successfully applied to the speciation analysis of mercury in the real samples with a recovery range of 90.3-110.3%.
Chapter four: A method has been described for the simultaneous determination of As(III), As(V), Sb(III) and Sb(V) in Traditional Chinese Medicines by hydride generation-double channel atomic fluorescence spectrometry. The experimental conditions that influence the fluorescence intensities of arsenic and antimony were
investigated and optimized, and the influence from foreign ions and the eliminations were studied. The detection limits were found to be 90.31 ng/L and 57.82 ng/L for arsenic and antimony, respectively. The proposed method was applied to the determination of arsenic and antimony species in seven kinds of Traditional Chinese Medicines. Recoveries were in the ranges of 90.1%~105.0%, 89.2%~102.0%, 89.7%~102.0% and 90.3%~110.0% for As(III), As(V), Sb(III) and Sb(V), respectively.
Chapter five: A method has been described for the determination of arsenic species by hydride generation-atomic fluorescence spectrometry using separation technique with sulphhydryl cotton fiber (SCF). In a medium of 1 mol/L HC1, As(III) can be adsorbed by SCF and separated from As(V). The experimental conditions that influence the atomic fluorescence signal intensity and the reduction of As(V) were investigated and optimized. The influence from foreign ions and the elimination were studied. The detection limit of 64.31 ng/L, relative standard deviations of 1.12% and a recovery range of 90.2%~116.3% were obtained. The proposed method was applied to the speciation analysis of arsenic in five kinds of Traditional Chinese Medicines.
Chapter six: A method has been described for the simultaneous determination of mercury and arsenic by vapor generation-double channel atomic fluorescence spectrometry. The experimental conditions that influence the atomic fluorescence signal intensities of Hg and As were investigated and optimized. Thiourea-citric acid-ferric ion was selected as enhancement reagent. The influence from foreign ions and the elimination were studied. The detection limits of this method for Hg and As were of 21.10 ng/L and 103.1 ng/L, respectively. Relative standard deviations of 2.01% and 2.39% for Hg and As, respectively, were obtained under optimum conditions. The proposed method was applied to the determination of mercury an
第1章：文献综述。对氢化物发生-双道原子荧光光谱法的应用和中药中微量元素的形态分析研究进展进行了评述。共引用文献88篇。
第2章：建立了蒸气发生-原子荧光光谱法测定总汞含量的分析方法。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汞原子荧光强度的影响；提出用硫脲—柠檬酸—Fe~(3+)作为增感剂增强汞的荧光信号；探讨了共存离子对汞测定的干扰和消除方法。在最佳实验条件下，将本法成功应用于人参再造丸等6种中药样品中总汞含量的分析测定，方法的检出限为5.748μg／L，相对标准偏差为1.56％，回收率为90.4％～109.6％。
第3章：建立了蒸气发生-原子荧光光谱法测定中草药复方方剂原生药、残渣、悬浮态、可溶态无机汞和有机汞的方法。研究了仪器的工作条件、试剂浓度、增感剂对汞原子荧光强度的影响及有机汞的氧化条件，探讨了共存离子对汞测定的干扰和消除方法，利用本方法成功地对万氏牛黄清心方剂中的汞进行了形态分析。方法检出限为7.611 ng／L，RSD为1.24％，回收率为90.3％-110.3％。
第4章：建立了一种氢化物发生-双道原子荧光光谱法同时测定中药中As(Ⅲ)、As(Ⅴ)、Sb(Ⅲ)和Sb(Ⅴ)的方法。研究了仪器的工作条件、试剂浓度对砷和锑原子荧光强度的影响以及五价砷、五价锑的还原条件，探讨了共存离子对砷和锑测定的干扰和消除方法。在最佳工作条件下，砷和锑的最低检出限分别为90.31ng／L和57.82ng／L，相对标准偏差分别为2.01％和1.39％。将本法成功应用于板蓝根颗粒等7种中药样品中砷和锑的形态分析，As(Ⅲ)和As(Ⅴ)的回收率分别为90.1％～105.0％和89.2％～102.0％，Sb(Ⅲ)和Sb(Ⅴ)的回收率分别为89.7％～102.0％和90.3％～110.0％。
第5章：建立了巯基棉分离吸附-氢化物发生-原子荧光光谱法测定中药中As(Ⅲ)和As(Ⅴ)的方法。在1mol／L盐酸介质中，巯基棉定量吸附As(Ⅲ)，不吸附As(Ⅴ)，
摘要
实现了As(III)和As(v)的分离。研究了仪器的工作条件、试剂浓度及不同增感剂对
砷原子吸收信号强度的影响和砷(V)的还原条件，探讨了共存离子对砷测定的干扰
和消除方法，利用本方法成功地对牛黄清火丸等5种中成药中的砷进行了形态分
析。方法检出限为64.3 ing几，RsD为1.120，0，回收率为90.2%一116.30，0。
第6章:建立了一种蒸气发生一双道原子荧光光谱法同时测定中药中汞和砷的
方法，考察并优化了影响荧光强度的实验条件;提出用硫脉一柠檬酸一Fe3+作为增感
剂增强汞和砷的荧光信号;探讨了共存离子对汞和砷测定的干扰及消除方法。在
最佳工作条件下，汞和砷的最低检出限分别为21 .10ng/L和103.Ing/L，相对标准
偏差分别为2.01%和2.39%。将本法成功应用于牛黄清胃丸等6种中药样品中汞和
砷的测定，汞和砷的回收率分别为90.7%一1 10.6%和91.2%一108.5%。
The studies of speciation analysis of mercury, arsenic and antimony in Traditional Chinese Medicine by atomic fluorescence spectrometry are described in this disertation, which consists of six chapters.
Chapter one: The recent progress of the application of hydride generation-double channel atomic fluorescence spectrometry and the speciation analysis of elements in Traditional Chinese Medicine has been reviewed with the relative references of 88.
Chapter two: A method has been described for the determination of mercury by vapor generation-atomic fluorescence spectrometry. The experimental conditions that influence the atomic fluorescence signal intensity were investigated and optimized, and the influence from foreign ions and the elimination were studied. Thiourea-citric acid-ferrite ion was selected as enhancement reagent. The detection limit and relative standard deviation were of 5.748jj,g/L and 1.56 %, respectively. The proposed method was applied to the determination of mercury in six kinds of Traditional Chinese Medicines with a recovery range of 90.4-109.6%.
Chapter three: A sensitive method has been proposed for the determination of inorganic mercury and total organic mercury in Traditional Chinese Medicine by vapor generation-atomic fluorescence spectrometry. The experimental conditions that influence the atomic fluorescence signal intensity of Hg and the oxidization of organic mercury were investigated and optimized. Thiourea-citric acid was selected as sensitization reagent. The influence from foreign ions and their elimination were studied. The detection limit of the method for Hg was of 7.611 ng/L and the relative standard deviation was 1.24%. The proposed method was successfully applied to the speciation analysis of mercury in the real samples with a recovery range of 90.3-110.3%.
Chapter four: A method has been described for the simultaneous determination of As(III), As(V), Sb(III) and Sb(V) in Traditional Chinese Medicines by hydride generation-double channel atomic fluorescence spectrometry. The experimental conditions that influence the fluorescence intensities of arsenic and antimony were
investigated and optimized, and the influence from foreign ions and the eliminations were studied. The detection limits were found to be 90.31 ng/L and 57.82 ng/L for arsenic and antimony, respectively. The proposed method was applied to the determination of arsenic and antimony species in seven kinds of Traditional Chinese Medicines. Recoveries were in the ranges of 90.1%~105.0%, 89.2%~102.0%, 89.7%~102.0% and 90.3%~110.0% for As(III), As(V), Sb(III) and Sb(V), respectively.
Chapter five: A method has been described for the determination of arsenic species by hydride generation-atomic fluorescence spectrometry using separation technique with sulphhydryl cotton fiber (SCF). In a medium of 1 mol/L HC1, As(III) can be adsorbed by SCF and separated from As(V). The experimental conditions that influence the atomic fluorescence signal intensity and the reduction of As(V) were investigated and optimized. The influence from foreign ions and the elimination were studied. The detection limit of 64.31 ng/L, relative standard deviations of 1.12% and a recovery range of 90.2%~116.3% were obtained. The proposed method was applied to the speciation analysis of arsenic in five kinds of Traditional Chinese Medicines.
Chapter six: A method has been described for the simultaneous determination of mercury and arsenic by vapor generation-double channel atomic fluorescence spectrometry. The experimental conditions that influence the atomic fluorescence signal intensities of Hg and As were investigated and optimized. Thiourea-citric acid-ferric ion was selected as enhancement reagent. The influence from foreign ions and the elimination were studied. The detection limits of this method for Hg and As were of 21.10 ng/L and 103.1 ng/L, respectively. Relative standard deviations of 2.01% and 2.39% for Hg and As, respectively, were obtained under optimum conditions. The proposed method was applied to the determination of mercury an
引文
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