改良的高效液相色谱法测定尿中1-羟基芘  

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

作　　者：李晓华[1] 冷曙光[1] 郭君[1] 关蕾[1] 郑玉新[1] 

机构地区：[1]中国疾病预防控制中心职业卫生与中毒控制所,北京100050

出　　处：《卫生研究》2003年第6期616-617,共2页Journal of Hygiene Research

摘　　要：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。A method for determination of 1-hydroxypyrene in urin e 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 dichlorometh ane, separated on reverse phase C18 and detected by fluorescence detector. Inter nal standard method was applied for the quantification of 1-hydroxypyrene. The standard curve was linear over the range 10-500μg/L with a correlation coe fficient>0 999. The limit of detection and of quantification were 0 01ng(signa l to noise=3) and 1 0μg/L in urine, respectively. The recovery from the entire procedure was found to be 94 0% at 5μg/L and 99 5% at 20μg/L. The intra-da y RSD values were found to be 6 2%, and 5 8% at 5, and 20μg/L respectivel y (a ll at n =6). The inter-day RSD values were 7 5%, and 8 9% for 5, and 2 0μg /L, respectively (all at n =6). This method is sensitive, efficient and relia ble, and was successfully used for the determination of 1-hydroxypyrene in urin e of workers exposed to polycyclic aromatic hydrocarbon.

关 键 词：高效液相色谱法 碱水解 l-羟基芘 尿样检测 职业健康 

分 类 号：R446.12[医药卫生—诊断学] R135[医药卫生—临床医学]