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目的:完善和规范化二甲苯接触者尿中甲基马尿酸的高效液相色谱测定法,较好地分离甲基马尿酸的3种同分异构体。方法:采用waters反相C18柱,以甲醇+0.1%冰乙酸(33+67)为流动相,流速为0.7 ml/min,波长为230 nm。结果:甲基马尿酸的3种同分异构体在25μg/ml～1000μg/ml范围内线性良好,相关系数r为0.9995～0.9996,相对标准偏差为2.0%～9.6%,加标回收率为91.36%～101.36%,2-甲基马尿酸、3-甲基马尿酸和4-甲基马尿酸的最低检测浓度分别为0.47μg/ml、0.46μg/ml、0.41μg/ml;3-甲基马尿酸和4-甲基马尿酸的分离度达到要求。结论:该方法能够使3-甲基马尿酸和4-甲基马尿酸达到分离,方法学各项指标均符合职业卫生标准制定指南第五部分-生物材料中化学物质测定方法的相关要求,可用于职业接触二甲苯人群尿中甲基马尿酸的测定。
OBJECTIVE: To improve and standardize the HPLC method for determination of methyl hippuric acid in urine of xylene contactors, and to better separate the three isomers of methylhippuric acid. Methods: Waters reversed phase C18 column was used with mobile phase of methanol + 0.1% glacial acetic acid (33 + 67) at a flow rate of 0.7 ml / min and a wavelength of 230 nm. Results: The three isomers of methylhippuric acid showed a good linearity in the range of 25μg / ml ~ 1000μg / ml with a correlation coefficient of 0.9995 ~ 0.9996 and a relative standard deviation of 2.0% ~ 9.6%. The recoveries were 91.36% ~ 101.36%, the minimum detectable concentrations of 2-methyl hippuric acid, 3-methyl hippuric acid and 4-methyl hippuric acid were 0.47μg / ml, 0.46μg / ml and 0.41μg / The separation of kimacholic acid and 4-methyl hippuric acid meets the requirements. Conclusion: The method can separate 3-methyl hippuric acid and 4-methyl hippuric acid, and the methodological indicators are in accordance with the relevant requirements of the fifth part of the Guide to Occupational Health Standards - Determination of chemical substances in biomaterials, available Determination of methyl hippuric acid in the urine of occupational exposure xylene groups.