研究了三乙醇胺(TEA)水溶液在电解质作用下的相分离及其通过形成TEA-Fe3+配合物实现三乙醇胺相对Fe3+的萃取,萃取过程将萃取剂和萃取溶剂合二为一。同时还讨论了表面张力、溶液提升率对火焰原子吸收光谱法(FAAS)测定三乙醇胺相中铁的影...研究了三乙醇胺(TEA)水溶液在电解质作用下的相分离及其通过形成TEA-Fe3+配合物实现三乙醇胺相对Fe3+的萃取,萃取过程将萃取剂和萃取溶剂合二为一。同时还讨论了表面张力、溶液提升率对火焰原子吸收光谱法(FAAS)测定三乙醇胺相中铁的影响。建立了TEA-K2HPO4-H2O双水相萃取、FAAS测定铁的新方法:在试液中加入1 mL三乙醇胺(1+1)和5 g K2HPO4后以水定容为10 mL,离心分离后用FAAS测定三乙醇胺相中的铁。线性范围20~240μg/L,检出限6.1μg/L(S/N=3),已用于自来水和井水中铁的萃取。展开更多
乙醇-磷酸氢二钾双水相体系萃取细胞培养液中的山银花黄酮类化合物,用高效液相色谱法分析样品中的山银花黄酮类化合物的含量,色谱柱为C_(18),流动相为甲醇-水(50%∶50%v/v,用磷酸酸化至pH 4.0),流速1.0 m L/min,检测波长352 nm。结果表...乙醇-磷酸氢二钾双水相体系萃取细胞培养液中的山银花黄酮类化合物,用高效液相色谱法分析样品中的山银花黄酮类化合物的含量,色谱柱为C_(18),流动相为甲醇-水(50%∶50%v/v,用磷酸酸化至pH 4.0),流速1.0 m L/min,检测波长352 nm。结果表明,双水相萃取山银花黄酮上相乙醇,得到5个信号较强的化合物,其色谱行为与未经萃取的相同浓度山银花黄酮粗提物样品基本一致;萃取山银花黄酮粗提物细胞培养液样品获同样结果,表明乙醇-磷酸氢二钾双水相萃取结合液相色谱可检测细胞培养液中的山银花粗提物的黄酮化合物,该双水相能较好萃取并浓缩黄酮类化合物分配于上相乙醇中,有利于成分复杂、低浓度生物样品中待测化合物的分离、纯化、浓缩。展开更多
By comparing three sequential extraction procedures, a new optimized extraction scheme for the molybdenum association in environmental samples was proposed.Five operational steps were described as exchangeable(KH_2PO_...By comparing three sequential extraction procedures, a new optimized extraction scheme for the molybdenum association in environmental samples was proposed.Five operational steps were described as exchangeable(KH_2PO_4+K_2HPO_4: including water-soluble), associated with organic matter(NaOH), Fe–Mn oxides and/or carbonates(HCl), sulfides(H_2O_2) and residue(HNO_3+HF+H_2O_2). An optimized extraction scheme was compared with Tessier's procedure and the Commission of European Communities Bureau of Reference(BCR) was applied to black shales. Results showed Tessier's procedure gave the lowest concentration values for exchangeable molybdenum and the highest values for the residual molybdenum, which could not present the efficiency of the extraction reagents. BCR's procedure showed the highest values in oxidizable molybdenum and presented four fractions of molybdenum, which did not demonstrate the fractions of molybdenum in the black shales in detail. The optimized extraction scheme demonstrated a certain improvement on extraction efficiency over Tessier's procedure for the lowest residual molybdenum, and revealed more featured fraction information of molybdenum in black shales than BCR's. Therefore, after a comparison with other two extraction procedures, the optimized extraction scheme proved suitable for the molybdenum in black shales and it also showed an accurate determination of the molybdenum in the fractions and source of bioavailable Mo.展开更多
文摘研究了三乙醇胺(TEA)水溶液在电解质作用下的相分离及其通过形成TEA-Fe3+配合物实现三乙醇胺相对Fe3+的萃取,萃取过程将萃取剂和萃取溶剂合二为一。同时还讨论了表面张力、溶液提升率对火焰原子吸收光谱法(FAAS)测定三乙醇胺相中铁的影响。建立了TEA-K2HPO4-H2O双水相萃取、FAAS测定铁的新方法:在试液中加入1 mL三乙醇胺(1+1)和5 g K2HPO4后以水定容为10 mL,离心分离后用FAAS测定三乙醇胺相中的铁。线性范围20~240μg/L,检出限6.1μg/L(S/N=3),已用于自来水和井水中铁的萃取。
文摘乙醇-磷酸氢二钾双水相体系萃取细胞培养液中的山银花黄酮类化合物,用高效液相色谱法分析样品中的山银花黄酮类化合物的含量,色谱柱为C_(18),流动相为甲醇-水(50%∶50%v/v,用磷酸酸化至pH 4.0),流速1.0 m L/min,检测波长352 nm。结果表明,双水相萃取山银花黄酮上相乙醇,得到5个信号较强的化合物,其色谱行为与未经萃取的相同浓度山银花黄酮粗提物样品基本一致;萃取山银花黄酮粗提物细胞培养液样品获同样结果,表明乙醇-磷酸氢二钾双水相萃取结合液相色谱可检测细胞培养液中的山银花粗提物的黄酮化合物,该双水相能较好萃取并浓缩黄酮类化合物分配于上相乙醇中,有利于成分复杂、低浓度生物样品中待测化合物的分离、纯化、浓缩。
基金financially supported by the National Key Basic Research Program of China (2014CB238903)the Natural Science Foundation of China (41073017,41273029)the Opening Fund of State Key Laboratory of Environmental Geochemistry
文摘By comparing three sequential extraction procedures, a new optimized extraction scheme for the molybdenum association in environmental samples was proposed.Five operational steps were described as exchangeable(KH_2PO_4+K_2HPO_4: including water-soluble), associated with organic matter(NaOH), Fe–Mn oxides and/or carbonates(HCl), sulfides(H_2O_2) and residue(HNO_3+HF+H_2O_2). An optimized extraction scheme was compared with Tessier's procedure and the Commission of European Communities Bureau of Reference(BCR) was applied to black shales. Results showed Tessier's procedure gave the lowest concentration values for exchangeable molybdenum and the highest values for the residual molybdenum, which could not present the efficiency of the extraction reagents. BCR's procedure showed the highest values in oxidizable molybdenum and presented four fractions of molybdenum, which did not demonstrate the fractions of molybdenum in the black shales in detail. The optimized extraction scheme demonstrated a certain improvement on extraction efficiency over Tessier's procedure for the lowest residual molybdenum, and revealed more featured fraction information of molybdenum in black shales than BCR's. Therefore, after a comparison with other two extraction procedures, the optimized extraction scheme proved suitable for the molybdenum in black shales and it also showed an accurate determination of the molybdenum in the fractions and source of bioavailable Mo.