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%.

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.