农作物和中草药中痕量元素形态分布分析研究
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摘要
氢化物发生-原子荧光光谱法具有检出限低、灵敏度高和可同时进行多元素分析等特点在痕量和微量元素分析的工作中发挥着越来越重要的作用。本文主要研究利用氢化物发生-原子荧光光谱技术在测定中草药和农作物中的微量元素砷、硒、锡、锑的应用。
全文分为：
第一章：对氢化物发生-原子荧光光谱法的原理、历史、现状及新进展等情况进行了评述，并对其应用前景加以展望，引用文献50篇。
第二章：采用L-半胱氨酸做预还原剂，建立了氢化物发生-原子荧光法同时测定砷锑的新方法。成功地测定了环境水样和中草药样品中的总砷，砷(Ⅲ)，总锑和锑(Ⅲ)；并采用索氏提取技术和正辛醇-水萃取技术对砷、锑形态在中药中的分布特征进行了分析研究。
第三章 采用超生波辅助水提取技术，以盐酸羟胺作预还原剂，建立了氢化物发生原子荧光法同时测定砷、硒的方法，并用于枸杞子中的砷、硒的测定和形态分布特征研究。
第四章 以十二烷基磺酸钠(SDS)作增敏剂，建立了在弱酸性介质条件下氢化物发生原子荧光法测定土壤中痕量锡的新方法，并研究了在土壤-水稻系统中微量元素锡的富集和分布特征。
A method, hydride generation atomic fluorescence spectrometry, for the determination of trace elements places more and more role in many fields, for its low detection limit, high sensitivity and simultaneously detected many elements. This paper focuses on the application of hydride generation atomic fluorescence spectrometry in determination of arsenic, selenium, tin and antimony in Chinese herbs and cropper. The paper consists of four chapters.
In chapter 1, the fundamental principle, history and the application progress of atomic fluorescence spectrometry are reviewed .with 50 references.
In Chapter 2, A new method was developed for simultaneous determination of trace arsenic and antimony in water and Chinese herbal medicines by hydride generation-atomic fluorescence spectrometry with L-cysteine as the prereductant. A Soxhlet extraction system and a n-octanol-water extraction system were employed for speciation analysis and research of As and Se in Chinese herbs.
In Chapter 3, a new method was developed for simultaneous determination of trace arsenic and selenium in lycium barbarum L. by hydride generation atomic fluorescence spectrometry, with hydrochloric hydroxylamine as the prereductant. A ultrasonic extraction was employed for the speciation and distribution of arsenic and selenium.
In chapter 4, a new method is developed for the determination of trace tin in soil by hydride generation fluorescence spectrometry with sodium dodecanesulfonate (SDS) as the sensitizing reagent, the concentration and distribution of trace tin in soil-paddy system was investigated.
全文分为：
第一章：对氢化物发生-原子荧光光谱法的原理、历史、现状及新进展等情况进行了评述，并对其应用前景加以展望，引用文献50篇。
第二章：采用L-半胱氨酸做预还原剂，建立了氢化物发生-原子荧光法同时测定砷锑的新方法。成功地测定了环境水样和中草药样品中的总砷，砷(Ⅲ)，总锑和锑(Ⅲ)；并采用索氏提取技术和正辛醇-水萃取技术对砷、锑形态在中药中的分布特征进行了分析研究。
第三章 采用超生波辅助水提取技术，以盐酸羟胺作预还原剂，建立了氢化物发生原子荧光法同时测定砷、硒的方法，并用于枸杞子中的砷、硒的测定和形态分布特征研究。
第四章 以十二烷基磺酸钠(SDS)作增敏剂，建立了在弱酸性介质条件下氢化物发生原子荧光法测定土壤中痕量锡的新方法，并研究了在土壤-水稻系统中微量元素锡的富集和分布特征。
A method, hydride generation atomic fluorescence spectrometry, for the determination of trace elements places more and more role in many fields, for its low detection limit, high sensitivity and simultaneously detected many elements. This paper focuses on the application of hydride generation atomic fluorescence spectrometry in determination of arsenic, selenium, tin and antimony in Chinese herbs and cropper. The paper consists of four chapters.
In chapter 1, the fundamental principle, history and the application progress of atomic fluorescence spectrometry are reviewed .with 50 references.
In Chapter 2, A new method was developed for simultaneous determination of trace arsenic and antimony in water and Chinese herbal medicines by hydride generation-atomic fluorescence spectrometry with L-cysteine as the prereductant. A Soxhlet extraction system and a n-octanol-water extraction system were employed for speciation analysis and research of As and Se in Chinese herbs.
In Chapter 3, a new method was developed for simultaneous determination of trace arsenic and selenium in lycium barbarum L. by hydride generation atomic fluorescence spectrometry, with hydrochloric hydroxylamine as the prereductant. A ultrasonic extraction was employed for the speciation and distribution of arsenic and selenium.
In chapter 4, a new method is developed for the determination of trace tin in soil by hydride generation fluorescence spectrometry with sodium dodecanesulfonate (SDS) as the sensitizing reagent, the concentration and distribution of trace tin in soil-paddy system was investigated.
引文
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[2] G. R.Kingsley, Am. J. Med. Technol., 1951, 16:247-253
[3] V.Vasak, V.Sedivee, Collection Czechoslov Chem. Communs., 1952, 18:64-72
[4] W. Holak., Gas-sampling technique for arsenic determination by atomic absorption spectrophotometry, Anal. Chem., 1969, 41(12): 1712-1713
[5] B. L. Huang, Recent studies on inductively coupled plasma sample introduction-Hydride generation, Spectromica Acta, Part B, 1988, 43: 381-389
[6] P. Verrept, C. Vandecasteele, G. Windels and R. Dams, Use of a refractor plate for automatic background correction in electrothermal vaporization inductively Coupled plasma atomic emission spectrometry, Spectromica Acta, Part B, 1991, 46: 99-102
[7] X. W. Guo, X. M. Guo, Shanghai Enviromental Sciences, 1995, 375 (14): 28-31
[8] E. F. Dolton, A. Malanoski, At. Absorpt. Newsl., 1971, 10:92.
[9] K. C. Thompson, D. R. Thomerson, Analyst, 1974, 99: 595.
[10] H. C. Freeman, J. F. Uthe, At. Absorpt. Newsl.,1976, 13: 75.
[11] R. S. Braman, L. L. Justen, C. C. Foreback, Direct volatilization-spectral emission type detection system for nanogram amounts of arsenic and antimony, Anal.Chem., 1972, 44(13): 2195-2199.
[12] Ebdon L., Wilkinson J. R. Anal.The determination of arsenic and selenium in coal buy continuous flow hydride-generation atomic absorption spectrometry and atomic fluorescence spectrometry. Chim. Acta., 1987, 194:177.
[13] Guo T. Z, Liu M. Z., Schrader W. Use of flow injection hydride generation technique in non-dispersive atomic fluorescence spectrometry. J.Anal. At. Spectrom., 1992, 7(4): 667.
[14] 郭小伟，郭旭明。段续流动氢化物发生法在AAS／AFS中的应用。光谱学与光谱分析，1995，15(3)：97．
[15] 吕运开，孙汉文。尿中痕量碲测定的萃取—氢化物发生原子荧光光谱法。分析测试学报，2000，19(4)：24。
[16] 郭小伟，郭旭明．《分析化学进展》，王尔康主编，南京大学出版社，p．80，1994，10，南京
[17] Xiao-wei Guo, and Xu-ming Guo. Studies on the reaction between cadmium and potassium tetrahydroborate in aqueous solutions and its application in atomic fluorescence spectrometry. Anal. Chim. Acta, 1995, 310(2): 377-385
[18] Xiao-wei Guo, and Xu-ming Guo. Determination of cadmium at ultra-trace levels by cold vapor atomic absorption spectrometry. J. Anal. At. Spectrom., 1995,10(11): 987-991
[19] J. Cacho, I. Beltran, and C. Nerin. J. Anal. At. Spectrom., 1989,4(10): 661-663
[20] M. C. Valdés-Hevia y Temprano, M. R. Fernández de la Campa, and A. Sanz-Medel. Generation of volatile cadmium species with sodium tetrahydroborate "from organized media: Application to cadmium determination by induvtively coupled plasma atomic emission spectrometry. J. Anal. At. Spectrom., 1993,8(9): 847-852
[21] A. D'Ulivo, and Y. W. Chen. J. Anal. At. Spectrom., 1989, 4:319
[22] L. Ebdon, P. Goodall, S, J. Hill, P. Stockwell, and. J. Anal. At. Spectrom., 1993, 8:723
[23] 喻听，廖振环，江祖成．FI-HG-ICP-AES测定痕量镉的研究．武汉大学学报(自然科学版)，1997，43(6)：751-755．
[24] Aizpǘn Fernández B., Valdés-Hevia y Temprano M.C., Fernández de la Campa M.R., Sanz-Medel A.and Neil P., Determination of arsenic by inductively-coupled plasma atomic emission spectrometry enhanced by hydride generation from B organized media, Talanta, 1992, 39(11): 1517-1523
[25] onilla M, Rodriguez L and Cammara C. J. Anal. At. Spectrometry, 1987, 2:157
[26] Ure AM (1990) In: Alloway BJ (ed) Heavy metals in soils.Blackie, p71
[27]. Stemmer KL(1976) Pharm Ther A 1: 157
[28] Andreae MO (1983) In: Wong CS, Boyle E, Bruland KW, Burton JD, Goldberg ED(eds) Trace metals in sea water. Plenum Press, New York
[29] Shibata Y, Morita M. Anal. Sci., 1989,5:507-509
[30] Poison C J, Tattersal R N. Clinical Yoxicology. Pitman, London England, 1969:181-184
[31] Zhang X. Vanderbiesen V, Cubber A D, Vanholder R Clin. Chem., 1996, 42:1231-1233.
[32] Dodd M, Pergantis SA, Cullen WR, Li H, Eigendorf GK, Reimer K J, Analyst, 1996 121: 223.
[33] Burlo F, Guijarro I, Carbonell-Barrachina A A, Valer D, Martinez-Sanchez F. J. Agric. Food Chem., 1999,47:1247-1253.
[34] Carbonell-Barrachina A A,. Burlo F, Martinez-Sanchez F. J. Agric.. Food Chem, 1999,47: 2288-2294.
[35] Agget J, Aspell AC(1976) Analyst 101: 341.
[36] Andreae MO, Asmodé J-F, Foster P, Van't dack L (1982) Anal Chem 53: 1766.
[37] Yamamoto M, Urata K, Murashige K, Yamamoto I(1981).Spectrochim Acta 36B: 671.
[38] Campbell AT, Howard A (1989) Analytical Proceedings 26: 32.
[39] Nakahara T, Kikui N, Determination of trace concentrations of antimony by the introduction of stibine into an inductively-coupled plasma for atomic emission spectrometry, Acta Chim Acta 1 1985,172: 127-138.
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