Groeseneken D, Veulemans H, Masschelein R, Van Vlem E
Laboratory of Occupational Hygiene and Toxicology, K.U. Leuven, Belgium.
Int Arch Occup Environ Health. 1989;61(4):249-54. doi: 10.1007/BF00381422.
A sensitive and specific method for the determination in urine of alkoxyacetic acids, the metabolites of ethylene glycol monoalkyl ethers, was developed by combining the advantages of two previously described methods. The acids were determined gas chromatographically as their pentafluorobenzylesters. The alkylation with pentafluorobenzylbromide was performed after dissolving the dry residue of lyophilized urine in methanol. Quantitative derivatization was obtained when the urinary pH was adjusted to pH 7.0, when the reagent concentration was 5% v/v, and when the reaction mixture was heated at 90 degrees C for 3 h. Sample clean-up was performed by adding bidistilled water and the esters were extracted with methylene chloride with high yields (95%). Alkoxyacetic acid concentrations in the range of 0.1 to 200 mg/l could be determined with an average imprecision of +/- 3.5%.
结合之前描述的两种方法的优点，开发了一种灵敏且特异的测定尿液中乙二醇单烷基醚代谢产物烷氧基乙酸的方法。这些酸以其五氟苄酯的形式通过气相色谱法进行测定。将冻干尿液的干残渣溶解在甲醇中后，用五氟苄基溴进行烷基化反应。当尿液pH值调至7.0、试剂浓度为5% v/v且反应混合物在90℃加热3小时时，可实现定量衍生化。通过加入双蒸水进行样品净化，并用二氯甲烷萃取酯，萃取产率很高（95%）。可以测定浓度范围为0.1至200 mg/l的烷氧基乙酸，平均不精密度为±3.5%。
