Mushak P, Dessauer K, Walls E L
Environ Health Perspect. 1977 Aug;19:5-10. doi: 10.1289/ehp.77195.
Procedures for assessment of arsenic in soft tissue by use of flameless atomic absorption (FAA) and gas-liquid chromatography (GLC), have been evolved, with special emphasis on the analytical distinction among inorganic, monomethyl-, and dimethylarsenic in several oxidation states. The chemical bases for such speciation reside in several properties of the arsenicals under consideration: (1) pentavalent inorganic arsenic, methylarsonic, and cacodylic acid are not extracted from tissue matter made strongly acid with hydrochloric acid, while the corresponding trivalent forms (as halides) are extracted; (2) chloroform extracts of samples treated under reducing conditions (HCl-KI) retain organoarsenicals when these extracts are re-extracted with water, but do not when aqueous solutions of oxidants are employed; (3) reduced cacodylate (dimethylarsinous acid) is not detected in the graphite furnace of an FAA unit under conditions selected, while cacodylate can be so detected. For GLC studies, monomethyl- and dimethylarsenic are simultaneously measured as the diethyldithiocarbamate complexes with an instrument equipped for electron-capture detection and containing a glass column packed with silanized 5% OV-17 on Anakrom A.S.
已经开发出了使用无火焰原子吸收(FAA)和气相色谱(GLC)来评估软组织中砷的方法,特别强调了在几种氧化态下无机砷、一甲基砷和二甲基砷之间的分析区分。这种形态分析的化学基础在于所考虑的砷化合物的几个特性:(1)五价无机砷、甲基胂酸和卡可基酸不会从用盐酸调至强酸性的组织物质中被萃取出来,而相应的三价形式(作为卤化物)则会被萃取出来;(2)在还原条件(HCl-KI)下处理的样品的氯仿萃取物,当这些萃取物用水再次萃取时会保留有机砷化合物,但当使用氧化剂的水溶液时则不会;(3)在选定的条件下,在FAA装置的石墨炉中未检测到还原态的卡可基酸盐(二甲基次胂酸),而卡可基酸盐则可以被检测到。对于GLC研究,一甲基砷和二甲基砷作为二乙氨基二硫代甲酸盐络合物,使用配备电子捕获检测且装有在Anakrom A.S.上硅烷化的5% OV-17填充玻璃柱的仪器同时进行测量。