柱前衍生高效液相色谱法分离分析甲酚异构体  

Separation and Determination of Isomers of Cresol by HPLC with Precolumn Derivatization

作　　者：吕海涛[1] 孙家隆[1] 张栓红[1] 

机构地区：[1]青岛农业大学化学与药学院,青岛266109

出　　处：《理化检验（化学分册）》2010年第4期383-385,共3页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：山东省青岛市科技局课题(06-3-2-4-nsh)

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%。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-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^-5 mol·L^-1 for both of ocresyl acetate and m-cresyl acetate,and in the range of（0.03-2.25）×10^-5 mol·L^-1 for p-cresyl acetate,with their values of detection limit（3S/N） of 1.88×10^-5 mol·L^-1（for o- and m-cresyl acetate） and 1.13×10^-5 mol·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.

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 

分 类 号：O652.63[理学—分析化学]