【摘要】：背景 自20世紀(jì)30年代以來，五氯苯酚鈉(NaPCP)被用作殺菌劑、除草劑和木材防腐劑在全球范圍內(nèi)廣泛使用。在我國(guó)，NaPCP主要用于血防滅螺的藥物，長(zhǎng)江流域被廣泛用于血吸蟲病宿主釘螺的主要防治農(nóng)藥。NaPCP通過食物鏈的轉(zhuǎn)移、富集和放大作用，在不同層面對(duì)生物體造成損傷。NaPCP可通過皮膚、呼吸道、消化道等途徑進(jìn)入生物體，使其受到系統(tǒng)毒性、生殖發(fā)育毒性、內(nèi)分泌干擾、致癌、免疫毒性的影響。NaPCP的弱雌激素作用和改變酶功能作用影響生殖發(fā)育，并且干擾甲狀腺素的正常功能。NaPCP本身不具有毒性，代謝產(chǎn)物發(fā)揮毒效應(yīng)。本課題通過建立NaPCP在生物樣本（血液）中的檢測(cè)方法，旨在對(duì)NaPCP的代謝過程有全面系統(tǒng)的了解，為更深一步研究NaPCP的毒性創(chuàng)立研究基礎(chǔ)，具有一定的實(shí)驗(yàn)意義。 目的 運(yùn)用毛細(xì)管柱DB-35MS（30×0.25×0.25）色譜柱，，根據(jù)職業(yè)衛(wèi)生標(biāo)準(zhǔn)GBZ/T210.5-2008《生物材料中化學(xué)物質(zhì)測(cè)定方法》，篩選合適的色譜分析條件，建立五氯苯酚鈉在血液中的檢測(cè)方法，排除各種干擾因素。 方法 本方法使用硫酸將NaPCP酸化為PCP，正己烷萃取，碳酸鉀溶液反萃��；由于五氯苯酚本身的沸點(diǎn)高（310℃），難于氣化，用氣相色譜法測(cè)定需要將其衍生化，乙酸酐衍生為五氯苯乙酸酯（PCP-OAc），再用正己烷萃取，用氣相色譜方法檢測(cè)。 1.NaPCP測(cè)定中血液樣本前處理方法的建立 2.NaPCP氣相色譜法檢測(cè)參數(shù)的建立 3.加標(biāo)回收率測(cè)定 4.最低檢測(cè)濃度測(cè)定 5.血液中NaPCP含量的穩(wěn)定性分析 6.精密度測(cè)定 結(jié)果：PCP-OAc質(zhì)量濃度在2.5μg/kg～500μg/kg范圍內(nèi)有良好的線性關(guān)系，相關(guān)回歸系數(shù)r=0.9992，線性回歸方程為Y=136.45X-134.26；方法檢出限0.3μg/kg，檢測(cè)線性范圍加標(biāo)回收率76.7%～115.0%，RSD小于10%。 結(jié)論 本研究建立NaPCP在血液中的檢測(cè)方法，該方法有更高的靈敏度，其最低檢出濃度為0.3μg/kg，遠(yuǎn)低于SC/T3030-2006《水產(chǎn)品中五氯苯酚及其鈉鹽殘留量的測(cè)定氣相色譜法》中最低檢出限1.0μg/kg，回收率76.7%～115.0%，符合GBZ/T210.5-2008《職業(yè)衛(wèi)生標(biāo)準(zhǔn)制定指南第5部分：生物材料中化學(xué)物質(zhì)測(cè)定方法》中規(guī)定回收率＞75%的相關(guān)要求，并優(yōu)于SC/T3030-2006《水產(chǎn)品中五氯苯酚及其鈉鹽殘留量的測(cè)定氣相色譜法》中回收率70%~110%；選擇DB-35MS型毛細(xì)管柱選擇性好，分離效果好，峰形尖銳對(duì)稱，實(shí)現(xiàn)了血液中待測(cè)物質(zhì)PCP-OAc的完全分離。
[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

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