摘 要目的：本研究通过采用 Waters 系统初步探讨用高效液相色谱法测定尿中二噁英代谢物--4,5-二氯邻苯二酚（4,5-DCC）的方法，为今后开展人群生物样品中二噁英的代谢产物 4,5- 二氯邻苯二酚的水平的监测与评价建立可靠的方法。88976

方法：采用 Waters 系统，仪器包括美国 Waters 公司的 Waters1525 型高效液相色谱仪、 Waters 1525 型泵、Waters 2707 型自动进样器、Waters2998 型 PDA 光电二极管矩阵检测器、 Waters 液相色谱柱。软件处理系统为美国 Waters 公司的 Breeze2。流动相使用甲醇/乙酸/ 水=50/4/46，流速设定为 1。0ml/min。美国 Waters 公司的色谱柱为 Waters 碳 18（C18）色 谱柱(4。6mm*250mm i。d。, 5μm)。检测波长为 285nm 的荧光检测器。配制 4,5-二氯邻苯二 酚 0。625μg/mL-200μg/mL 标准系列对方法的线性范围、准确度、精密度及灵敏度进行测定。

尿样经过浓盐酸水解、两次乙醚萃取、甲醇定容、滤膜过滤后，用色谱柱分离，光电二 极管矩阵色谱检测器检测，最后用标准系列标准曲线定量。

结果：标准曲线线性范围是 0。625μg/mL -200。0μg/mL。尿样的检出限为 2。519μg/mL。 加标回收率为 55。65%；在连续 10 天内检测的尿样样品变异系数是 15。6%,浓度为 200。0μ g/mL 标准溶液的变异系数 0。0349%。标准曲线斜率质控图、2。5μg/mL 含量面积比质控图、 5。0μg/mL 含量面积比质控图所有数据均未超过三倍标准差，大部分数据接近平均值。

结论：本文探讨了采用 Waters 系统初步探讨用高效液相色谱法测定尿中二噁英代谢物--4,5-二氯邻苯二酚（4,5-DCC）的方法。该方法的线性范围为 0。625μg/mL -200。0μg/mL， 方法的精密度和稳定性均较好，但方法的准确度和尿样样品前处理方法有待改进。

关键词：高效液相色谱法； 4,5-二氯邻苯二酚； 尿源Q于D优G尔X论V文Y网wwW.yOueRw.com 原文+QQ75201`8766

AbstractObjective: In this study, the method of high performance liquid chromatography (HPLC) was used to determine the dioxin-metabolite-4,5- Dichlorocatechol (4,5-DCC) in urine by using Waters system。 The determination and evaluation of the level of metabolite 4,5- Dichlorocatechol in dioxins establishes a reliable method。

Method: Using the Waters system。Waters 1525, Waters Model 2707 Autosampler, Waters2998 PDA Photodiode Matrix Detector, Waters LC Columns, Waters Model 1525, Waters 1525, Waters, The software processing system is Breeze2 of Waters, USA。 The mobile phase was methanol / acetic acid / water = 50/4/46 and the flow rate was 1。0 ml / min。 Waters C18 (4。6mm * 250mm id, 5μm)。 Detection of wavelength detector 285nm。 Preparation of 4,5-dichloro-caffeine 0。625μg / mL-200μg

/ mL standard series of methods The linear range, accuracy, precision, and sensitivity were measured。

Urine samples after concentrated hydrochloric acid hydrolysis, two ether extraction, methanol quantitative volume, filter filter, separated by a column, photodiode matrix chromatographic detector detection, and finally with the standard series of standard curve quantitative。

Result: In this paper, we investigated the method of high performance liquid chromatography (HPLC) for the determination of dioxin - metabolite - 4,5- Dichlorocatechol (4,5 - DCC) in urine by using Waters system。 The linear range of the method is 0。625μg / mL -200。0μg / mL。 Standard curve slope control chart,  2。5μg

/ mL content area than the quality control map, 5。0μg / mL content area than the quality control map all data were not more than three times the standard deviation, most of the data close to the average。

Conclusion: In this paper, we investigated the method of high performance liquid chromatography (HPLC) for the determination of dioxin - metabolite - 4,5- Dichlorocatechol (4,5 - DCC) in urine by using Waters system。 The linear range of the method is 0。625μg / mL -200。0μg / mL。 The linear range of the method is 0。625μg