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微柱高效液相色谱法测定烟草样品中铁钴镍铜锌锰 被引量:23

MICRO-COLUMN HPLC DETERMINATION OF Fe Co Ni Cu Zn AND Mn IN TOBACCO
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摘要 研究了用2(2喹啉偶氮)5二甲氨基酚(QADMAP)为柱前衍生试剂,以Waters XterraTMRP18(1.0mm×50mm,2.5μm)微柱为固定相,72%的甲醇(内含0.5%的乙酸)为流动相,高效液相色谱法分离,二极管矩阵检测器检测测定铁、钴、镍、铜、锌和锰的方法。根据信噪比(S/N=3)得各金属离子的检出限分别为:铁3μg·L-1、钴和铜4μg·L-1、镍2μg·L-1、锌5μg·L-1、锰8μg·L-1,方法用于烟草中痕量铁、钴、镍、铜、锌和锰的测定,相对标准偏差在1.6%~3.8%之间,回收率在93%~107%之间,结果满意。 Quinolylazo) 5 dimethylaminophenol (QADMAP) was used as precolumn derivatizing reagent to form colored complexes with Fe(Ⅲ)、 Co(Ⅱ)、 Ni(Ⅱ)、 Cu(Ⅱ)、 Zn(Ⅱ) and Mn(Ⅱ) in weakly acidic medium (pH 2.8~6.2). For the separation of the above mentioned complexes, the Waters Xterra RP 18 micro column (1.0 mm ×50 mm, 2.5 μm) was used as stationary phase, and a mixture of methanol and water (CH 3OH+H 2O=72+28 by volume, containing 0.5% by volume of acetic acid) was used as mobile phase. Optimum HPLC conditions were studied and described in detail. Array diodes were used in the determination. Detection limits ( S/N =3) of these metal complexes were found to be 3 μg·L -1 for Fe(Ⅲ), 4 μg·L -1 for Co(Ⅱ), 2 μg·L -1 for Ni(Ⅱ), 4 μg·L -1 for Cu(Ⅱ), 5 μg·L -1 for Zn(Ⅱ) and 8 μg·L -1 for Mn(Ⅱ). In its application to the analysis of tobacco samples, RSD′s in the range of 1.6%~3.8%, and recoveries in the range of 93%~107%, were obtained.
出处 《理化检验(化学分册)》 CAS CSCD 北大核心 2005年第4期235-237,共3页 Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
关键词 高效液相色谱法 2-(2-喹啉偶氮)-5-二甲氨基酚 烟草 HPLC 2 (2 Quinolylazo) 5 dimethylaminophenol Tobacco Iron(Ⅲ) Nickel(Ⅱ) Cobalt(Ⅱ) Copper(Ⅱ) Zinc(Ⅱ) Manganese(Ⅱ)
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