Gori G, Bartolucci G B, Sturaro A, Parvoli G, Doretti L, Troiano R, Casetta B
Istituto di Medicina del Lavoro, Università di Padova, Italy.
J Chromatogr B Biomed Appl. 1995 Nov 17;673(2):165-72. doi: 10.1016/0378-4347(95)00257-x.
The good correlation between exposure to n-hexane and 2,5-hexanedione urinary excretion confers on this diketone an important toxicological meaning. this paper proposes a reversed-phase HPLC method which includes, after acid hydrolysis, a derivatization step of 2,5-hexanedione with 2,4-dinitrophenylhydrazine at 70 degrees C for 20 min. The reaction conditions, such as temperature, reagent concentration and time, are optimized so as to allow the condensation of a single carbonyl group. A linear response was obtained in the 0.19-20.0 mg/l range with a detection limit of 0.03 mg/l, corresponding to a signal-to-noise ratio of 3. A phosphate buffer (pH 3.3)-acetonitrile mixture (50:50) as the eluent and UV detection at 334 nm were used.
接触正己烷与尿中2,5 - 己二酮排泄之间的良好相关性赋予了这种二酮重要的毒理学意义。本文提出了一种反相高效液相色谱法，该方法包括在酸性水解后，2,5 - 己二酮与2,4 - 二硝基苯肼在70℃下衍生化20分钟的步骤。对反应条件，如温度、试剂浓度和时间进行了优化，以实现单个羰基的缩合。在0.19 - 20.0 mg/L范围内获得了线性响应，检测限为0.03 mg/L，对应信噪比为3。使用磷酸盐缓冲液（pH 3.3）-乙腈混合物（50:50）作为洗脱液，并在334 nm处进行紫外检测。
