五氯苯酚钠在血液中的检测方法研究
发布时间：2018-08-23 14:30
【摘要】：背景 自20世纪30年代以来，五氯苯酚钠(NaPCP)被用作杀菌剂、除草剂和木材防腐剂在全球范围内广泛使用。在我国，NaPCP主要用于血防灭螺的药物，长江流域被广泛用于血吸虫病宿主钉螺的主要防治农药。NaPCP通过食物链的转移、富集和放大作用，在不同层面对生物体造成损伤。NaPCP可通过皮肤、呼吸道、消化道等途径进入生物体，使其受到系统毒性、生殖发育毒性、内分泌干扰、致癌、免疫毒性的影响。NaPCP的弱雌激素作用和改变酶功能作用影响生殖发育，并且干扰甲状腺素的正常功能。NaPCP本身不具有毒性，代谢产物发挥毒效应。本课题通过建立NaPCP在生物样本（血液）中的检测方法，旨在对NaPCP的代谢过程有全面系统的了解，为更深一步研究NaPCP的毒性创立研究基础，具有一定的实验意义。 目的 运用毛细管柱DB-35MS（30×0.25×0.25）色谱柱，，根据职业卫生标准GBZ/T210.5-2008《生物材料中化学物质测定方法》，筛选合适的色谱分析条件，建立五氯苯酚钠在血液中的检测方法，排除各种干扰因素。 方法 本方法使用硫酸将NaPCP酸化为PCP，正己烷萃取，碳酸钾溶液反萃取；由于五氯苯酚本身的沸点高（310℃），难于气化，用气相色谱法测定需要将其衍生化，乙酸酐衍生为五氯苯乙酸酯（PCP-OAc），再用正己烷萃取，用气相色谱方法检测。 1.NaPCP测定中血液样本前处理方法的建立 2.NaPCP气相色谱法检测参数的建立 3.加标回收率测定 4.最低检测浓度测定 5.血液中NaPCP含量的稳定性分析 6.精密度测定 结果：PCP-OAc质量浓度在2.5μg/kg～500μg/kg范围内有良好的线性关系，相关回归系数r=0.9992，线性回归方程为Y=136.45X-134.26；方法检出限0.3μg/kg，检测线性范围加标回收率76.7%～115.0%，RSD小于10%。 结论 本研究建立NaPCP在血液中的检测方法，该方法有更高的灵敏度，其最低检出浓度为0.3μg/kg，远低于SC/T3030-2006《水产品中五氯苯酚及其钠盐残留量的测定气相色谱法》中最低检出限1.0μg/kg，回收率76.7%～115.0%，符合GBZ/T210.5-2008《职业卫生标准制定指南第5部分：生物材料中化学物质测定方法》中规定回收率＞75%的相关要求，并优于SC/T3030-2006《水产品中五氯苯酚及其钠盐残留量的测定气相色谱法》中回收率70%~110%；选择DB-35MS型毛细管柱选择性好，分离效果好，峰形尖锐对称，实现了血液中待测物质PCP-OAc的完全分离。
[Abstract]:Background since the 1930s, sodium pentachlorophenol (NaPCP) has been widely used as fungicides, herbicides and wood preservatives worldwide. In China, NaPCP is mainly used to prevent and control snails, and the Yangtze River valley is widely used to control snails, which is the host of schistosomiasis. NaPCP is widely used to prevent and control snails from schistosomiasis through food chain transfer, enrichment and amplification. In different levels of damage to organisms. NaPCP can be through the skin, respiratory, digestive tract and other ways to enter the organism, so that it is subject to systemic toxicity, reproductive development toxicity, endocrine disruption, carcinogenesis, Effects of immunotoxicity. Weak estrogenic effect of NaPCP and alteration of enzyme function affect reproductive development, and interfere with the normal function of thyroxine. NaPCP is not toxic, and metabolites play a toxic role. The purpose of this study is to establish a method for the detection of NaPCP in biological samples (blood) in order to have a comprehensive and systematic understanding of the metabolic process of NaPCP, and to establish the foundation for further study on the toxicity of NaPCP, which is of certain experimental significance. Objective to establish a capillary column DB-35MS column (30 脳 0.25 脳 0.25) for the determination of sodium pentachlorophenol in blood according to occupational hygiene standard GBZ/T210.5-2008 < method for determination of chemical substances in biomaterials]. Eliminate all kinds of interference. Methods NaPCP was acidified by sulfuric acid, extracted by n-hexane, and reextracted by potassium carbonate solution. Because of its high boiling point (310 鈩
本文编号：2199354
[Abstract]:Background since the 1930s, sodium pentachlorophenol (NaPCP) has been widely used as fungicides, herbicides and wood preservatives worldwide. In China, NaPCP is mainly used to prevent and control snails, and the Yangtze River valley is widely used to control snails, which is the host of schistosomiasis. NaPCP is widely used to prevent and control snails from schistosomiasis through food chain transfer, enrichment and amplification. In different levels of damage to organisms. NaPCP can be through the skin, respiratory, digestive tract and other ways to enter the organism, so that it is subject to systemic toxicity, reproductive development toxicity, endocrine disruption, carcinogenesis, Effects of immunotoxicity. Weak estrogenic effect of NaPCP and alteration of enzyme function affect reproductive development, and interfere with the normal function of thyroxine. NaPCP is not toxic, and metabolites play a toxic role. The purpose of this study is to establish a method for the detection of NaPCP in biological samples (blood) in order to have a comprehensive and systematic understanding of the metabolic process of NaPCP, and to establish the foundation for further study on the toxicity of NaPCP, which is of certain experimental significance. Objective to establish a capillary column DB-35MS column (30 脳 0.25 脳 0.25) for the determination of sodium pentachlorophenol in blood according to occupational hygiene standard GBZ/T210.5-2008 < method for determination of chemical substances in biomaterials]. Eliminate all kinds of interference. Methods NaPCP was acidified by sulfuric acid, extracted by n-hexane, and reextracted by potassium carbonate solution. Because of its high boiling point (310 鈩
本文编号：2199354
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