Separation and Determination of Isomers of Cresol by HPLC with Precolumn Derivatization
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-C18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260 nm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)×10-5mol·L-1范围内呈线性关系,而乙酸对甲酚酯在(0.03~2.25)×10-5mol·L-1之间呈线性关系,检出限(3S/N)依次为1.88×10-5,1.88×10-5,1.13×10-5mol·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%.
Abstract
Method for separation and determination of o-cresol,m-cresol and p-cresol by HPLC with pre-column 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-C18 column was used as the separation column,and a mixture of methanol and water (35+65,by vol.) was used as eluent in the separation.UV-detection at 260 nm was used in the determination.Linear relationships were kept between values of peak area and concentration in the range of (0.05-3.75)×10-5mol·L-1 for both of o-cresyl acetate and m-cresyl acetate,and in the range of (0.03-2.25)×10-5mol·L-1 for p-cresyl acetate,with their values of detection limit (3S/N) of 1.88×10-5mol·L-1 (for o- and m-cresyl acetate) and 1.13×10-5mol·L-1 (for p-cresyl acetate).Recovery of the method was tested by standard addition method using samples of o-,m- and p-cresol as matrixes,values of average recovery found were 104%,95% and 100% with values of RSD (n=7) of 0.22%,2.34% and 0.90% respectively.
中图分类号 O652.63
所属栏目 工作简报
基金项目 山东省青岛市科技局课题(06-3-2-4-nsh)
收稿日期 2009/1/22
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备注吕海涛(1968-),男,山东烟台人,教授,博士,主要从事色谱分析和天然产物活性物质提取方面的研究.
引用该论文: Lv Hai-tao,SUN Jia-long,ZHANG Shuan-hong. Separation and Determination of Isomers of Cresol by HPLC with Precolumn Derivatization[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2010, 46(4): 383~385
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, 46(4): 383~385
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【3】陶旦妮,史雪岩,顾峻岭,等.环糊精衍生物固定相毛细管气相色谱法分离甲酚位置异构体[J].分析化学,2001,29(10):1150-1153.
【4】张月琴,史雪岩,傅若农,等.毛细管气相色谱法分析苯酚和甲酚位置异构体[J].北京理工大学学报,2000,20(3):380-384.
【5】唐新德,张其展,侯昭升,等.偶氮苯和胆甾酯侧链聚硅氧烷高分子液晶固定液色谱分离二氯苯和甲酚异构体[J].化学分析计量,2002,11(6):21-22.
【6】谢复炜,赵明月,王昇,等.卷烟主流、侧流烟气中酚类化合物的高效液相色谱测定[J].烟草科技,2004(5):6-10.
【7】宣栋梁,黎源倩.高效液相色谱法测定环境水中的酚类化合物[J].中国公共卫生,2002,18(9):1102-1104.
【8】黄云,樊瑛,缪明明,等.用快速分离柱高效液相色谱法测定烟草中的几种酚[J].分析试验室,2007,26(8):8-13.
【9】李慧章,刘卉闵,肖立伟.微波辐射下快速合成乙酸酚酯[J].河北大学学报,2003,23(3):262-264.
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