改良的高效液相色谱法测定尿中1-羟基芘

改进并规范了尿中 1 羟基芘的碱水解 -高效液相色谱分析方法。尿样经碱水解、二氯甲烷提取后 ,用反相柱分离 ,荧光检测器检测。内标标准曲线法定量。标准曲线线性范围 10～ 50 0 μg L。尿样加标的检出限 (三倍噪声 )为 0 0 1ng ,定量限为 1 0 μg L尿。高、低两个浓度下的回收率分别为 99 5%和 94 0 % ;天内精密度为 5 8%和 6 2 % (RSD) ;天间精密度为 7 7%和 8 9% (RSD)。该方法可用于测定接触多环芳烃人群的尿中 1 羟基芘 ,具有快速简便、准确可靠的特点

An improved high performance liquid chromatography method for determination of 1-hydroxypyrene in urine

A method for determination of 1-hydroxypyrene in urine by alkaline hydrolysis and high performance liquid chromatography was improved and validated. The conjugated 1-hydroxypyrene in urine samples was decomposed by sodium hydroxide. The urinary 1-hydroxypyrene were extracted by dichloromethane, separated on reverse phase C18 and detected by fluorescence detector. Internal standard method was applied for the quantification of 1-hydroxypyrene. The standard curve was linear over the range 10-500 micrograms/L with a correlation coefficient > 0.999. The limit of detection and of quantification were 0.01 ng(signal to noise = 3) and 1.0 microgram/L urine, respectively. The recovery from the entire procedure was found to be 94.0% at 5 micrograms/L and 99.5% at 20 micrograms/L. The intra-day RSD values were found to be 6.2%, and 5.8% at 5, and 20 micrograms/L respectively (all at n = 6). The inter-day RSD values were 7.5%, and 8.9% for 5, and 20 micrograms/L, respectively (all at n = 6). This method is sensitive, efficient and reliable, and was successfully used for the determination of 1-hydroxypyrene in urine of workers exposed to polycyclic aromatic hydrocarbon.