微乳高效液相色谱法同时测定多种金属离子
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摘要
本文建立了一种以4 -(2-吡啶偶氮)间苯二酚(PAR)为柱前衍生试剂,微乳液高效液相色谱法测定Fe~(3+)、Co~(2+)、Ni~(2+)离子的方法。实验得到的最佳条件是:色谱柱ODS-2 Hypersil(200 mm×4.6 mm),流动相为微乳液[十六烷基三甲基溴化铵(CTMAB)0.6 g+正丁醇1.3 g+正庚烷0.1 g+水100 g](含20 mmol/L Na2HPO4-KH2PO4缓冲溶液)/甲醇25:75(体积比),在室温条件下,流速1.0 mL/min,检测波长530 nm。
实验结果表明:在微乳液存在的条件下,在确定的最佳柱前衍生条件和色谱测定条件下,Fe~(3+)、Co~(2+)、Ni~(2+)离子配合物在10 min内能够完全分离,灵敏度分别提高了90.38%、45.68%、32.45%。线性范围分别为Fe~(3+) 0.1μg/mL ~1.1μg/mL,Co~(2+) 0.015μg/mL~1.2μg/mL,Ni~(2+) 0.02μg/mL~0.6μg/mL;检出限分别为Fe~(3+) 23.42μg/L、Co~(2+) 9.69μg/L、Ni~(2+)10.76μg/L。方法应用于环境水样和中药样品的分析测定中,相对标准偏差在1.76%~3.96%之间,回收率在94.5%~101.3%之间;并利用原子吸收光度法对样品进行测定,两种实验方法没有显著性差异。
用电导率法结合微乳液的结构理论讨论了含水量、pH值和温度对微乳液的结构的影响,并结合色谱分离条件对3种离子的色谱行为进行了说明。
Determination of iron(Ⅲ)、Cobalt(Ⅱ) and Nickel(Ⅱ)in environment with PAR as precolumn derivatization reagent by microemusion liquid chromatography was studied. The optimal conditions as follows: the flow rate of 1.0 mL / min, at 530nm, a ODS-2 Hypersil column(200 mm×4.6 mm)used at room temperature, the mobile phase is microemulsion consisted of CTMAB 0.6 g,n-butanol 1.3g, n-heptane 0.1g, water 100g(containing 20mmol / L Na2HPO4-KH2PO4 buffer solution)/methanol 25:75(v/v).
The results show that: in the optimal precolumn derived and chromatographic conditions containing microemulsion,Fe(Ⅲ)、Co(Ⅱ)、Ni(Ⅱ) complexes can be completely separated within 10 min, the sensibility has respectively improved 90.38%、45.68%、32.45%.The linear rang is respectively 0.1~1.1μg/mL for Fe~(3+),0.015~1.2μg/mL for Co~(2+) and 0.02~0.6 for Ni~(2+); the detection limit is respectively 23.42μg / L for Fe~(3+), 9.69μg / L for Co~(2+) and 10.76μg / L for Ni~(2+). The proposed method has been successfully applied to the determination of Fe、Co、Ni in water samples and traditional Chinese medicine, the relative standard deviations are 1.76% ~ 3.96%, the recovery is among 94.5% ~ 101.3%; compared with AAS, the two methods have no prominently difference.
The influence on the structure of microemulsion through changing the water content, pH, and temperature basedon the conductivity and microemulsion structure theory, combined with chromatographic separation conditions on chromatographic behavior of three kinds of ions was further explained.
实验结果表明:在微乳液存在的条件下,在确定的最佳柱前衍生条件和色谱测定条件下,Fe~(3+)、Co~(2+)、Ni~(2+)离子配合物在10 min内能够完全分离,灵敏度分别提高了90.38%、45.68%、32.45%。线性范围分别为Fe~(3+) 0.1μg/mL ~1.1μg/mL,Co~(2+) 0.015μg/mL~1.2μg/mL,Ni~(2+) 0.02μg/mL~0.6μg/mL;检出限分别为Fe~(3+) 23.42μg/L、Co~(2+) 9.69μg/L、Ni~(2+)10.76μg/L。方法应用于环境水样和中药样品的分析测定中,相对标准偏差在1.76%~3.96%之间,回收率在94.5%~101.3%之间;并利用原子吸收光度法对样品进行测定,两种实验方法没有显著性差异。
用电导率法结合微乳液的结构理论讨论了含水量、pH值和温度对微乳液的结构的影响,并结合色谱分离条件对3种离子的色谱行为进行了说明。
Determination of iron(Ⅲ)、Cobalt(Ⅱ) and Nickel(Ⅱ)in environment with PAR as precolumn derivatization reagent by microemusion liquid chromatography was studied. The optimal conditions as follows: the flow rate of 1.0 mL / min, at 530nm, a ODS-2 Hypersil column(200 mm×4.6 mm)used at room temperature, the mobile phase is microemulsion consisted of CTMAB 0.6 g,n-butanol 1.3g, n-heptane 0.1g, water 100g(containing 20mmol / L Na2HPO4-KH2PO4 buffer solution)/methanol 25:75(v/v).
The results show that: in the optimal precolumn derived and chromatographic conditions containing microemulsion,Fe(Ⅲ)、Co(Ⅱ)、Ni(Ⅱ) complexes can be completely separated within 10 min, the sensibility has respectively improved 90.38%、45.68%、32.45%.The linear rang is respectively 0.1~1.1μg/mL for Fe~(3+),0.015~1.2μg/mL for Co~(2+) and 0.02~0.6 for Ni~(2+); the detection limit is respectively 23.42μg / L for Fe~(3+), 9.69μg / L for Co~(2+) and 10.76μg / L for Ni~(2+). The proposed method has been successfully applied to the determination of Fe、Co、Ni in water samples and traditional Chinese medicine, the relative standard deviations are 1.76% ~ 3.96%, the recovery is among 94.5% ~ 101.3%; compared with AAS, the two methods have no prominently difference.
The influence on the structure of microemulsion through changing the water content, pH, and temperature basedon the conductivity and microemulsion structure theory, combined with chromatographic separation conditions on chromatographic behavior of three kinds of ions was further explained.
引文
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