Chen Jing-Huan, Jiang Shiuh-Jen
Department of Chemistry, National Sun Yat-sen University, Kaohsiung, Taiwan.
J Agric Food Chem. 2008 Feb 27;56(4):1210-5. doi: 10.1021/jf073213h. Epub 2008 Feb 2.
A capillary electrophoresis-inductively coupled plasma mass spectrometric (CE-ICP-MS) method for the determination of cobalamin is described. Samples of cobalt-containing compounds were subjected to electrophoretic separation before injection into the microconcentric nebulizer (CEI-100) of ICP-MS. The Co-containing compounds studied include cyanocobalamin (CN-Cbl, vitamin B12), hydroxocobalamin (OH-Cbl), and Co(II). The species studied were well separated using a 70 cm lengthx75 microm i.d. fused silica capillary with the applied voltage set at +20 kV. A 25 mM Tris buffer (pH 9.0) containing 15 mM sodium dodecyl sulfate (SDS) was used as the electrophoretic buffer. The CE-ICP-MS detection limits were 0.3, 0.2, and 1.7 ng of Co mL(-1) for CN-Cbl, OH-Cbl, and Co(II), respectively. The concentrations of cobalamin compounds were determined in selected nutritive supplements and chlorella samples. A microwave-assisted extraction method was used for the extraction of these compounds. Over 92% of the total cobalt species was extracted using a 5% v/v HNO3 solution in a focused microwave field within a period of 10 min; spike recovery was in the range of 94-105% for various species. The major cobalt species in nutritive supplements and chlorella samples was cyanocobalamin.
描述了一种用于测定钴胺素的毛细管电泳-电感耦合等离子体质谱法(CE-ICP-MS)。含钴化合物样品在注入ICP-MS的微同心雾化器(CEI-100)之前先进行电泳分离。所研究的含钴化合物包括氰钴胺(CN-Cbl,维生素B12)、羟钴胺(OH-Cbl)和Co(II)。使用一根长度为70 cm、内径为75 μm的熔融石英毛细管,在+20 kV的施加电压下,所研究的物种得到了很好的分离。以含有15 mM十二烷基硫酸钠(SDS)的25 mM Tris缓冲液(pH 9.0)作为电泳缓冲液。CE-ICP-MS对CN-Cbl、OH-Cbl和Co(II)的检测限分别为0.3、0.2和1.7 ng Co mL(-1)。在选定的营养补充剂和小球藻样品中测定了钴胺素化合物的浓度。采用微波辅助萃取法萃取这些化合物。在聚焦微波场中,使用5% v/v HNO3溶液在10分钟内可萃取超过92%的总钴物种;各种物种的加标回收率在94-105%范围内。营养补充剂和小球藻样品中的主要钴物种是氰钴胺。