| 柱前衍生高效液相色谱法分离分析甲酚异构体 |
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| 引用本文： | 吕海涛,孙家隆,张栓红.柱前衍生高效液相色谱法分离分析甲酚异构体[J].理化检验(化学分册),2010(4). |
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| 作者姓名： | 吕海涛 孙家隆 张栓红 |
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| 作者单位： | 青岛农业大学化学与药学院; |
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| 基金项目： | 山东省青岛市科技局课题(06-3-2-4-nsh) |
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| 摘 要： | 提出了柱前衍生高效液相色谱法同时分离测定邻甲酚、间甲酚和对甲酚的方法。含甲酚异构体的样品与衍生化试剂按1比8(质量比)混合,加热回流衍生2 h。3种异构体的转化率依次为98.1%,99.0%,98.5%。选用Eclipse XDB-C_(18)色谱柱作为反相色谱柱,以甲醇和水以体积比为35比65的混合溶液为流动相,在260nm波长处进行测定,乙酸邻甲酚酯、乙酸间甲酚酯的峰面积与其浓度在(0.05～3.75)×10~(-5)mol·L~(-1)范围内呈线性关系,而乙酸对甲酚酯在(0.03～2.25)×10~(-5)mol·L~(-1)之间呈线性关系,检出限(3S/N)依次为1.88×10~(-5),1.88×10~(-5),1.13×10~(-5)mol·L~(-1)。此方法应用于实际样品的测定,回收率分别为104%,95%,100%,相对标准偏差(n=7)分别为0.22%,2.34%,0.90%。
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| 关 键 词： | 高效液相色谱法 柱前衍生 邻甲酚 间甲酚 对甲酚 乙酸酐 |
Separation and Determination of Isomers of Cresol by HPLC with Precolumn Derivatization |
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| Institution: | College of Chemistry and Pharmacy/a>;Qingdao Agricultural University/a>;Qingdao 266109/a>;China |
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| Abstract: | Method for separation and determination of o-cresol,m-cresol and p-cresol by HPLC with precolumn derivatization with acetic anhydride as derivatizing agent was proposed.Sample containing isomers of cresol was mixed with acetic anhydride with mass ratio of 1 to 8,and refluxed under heating for 2 h,giving values of yield of 98.1%,99.0%and 98.5%for o-cresyl acetate,m-cresyl acetate and p-cresyl acetate respectively.The Eclipse XDB-C_(18) column was used as the separation column,and a mixture of methanol and wa... |
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| Keywords: | HPLC Pre-column derivatization o-Cresol m-Cresol p-Cresol Acetic anhydride |
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