本文選題：糖皮質(zhì)激素 + 地表水��； 參考：《南京師范大學(xué)》2015年碩士論文

【摘要】：內(nèi)分泌干擾物質(zhì)(EDCs)因其在低濃度下干擾生物機體的內(nèi)分泌系統(tǒng)正常功能而備受研究者關(guān)注,與雌激素相比,種類繁多的糖皮質(zhì)激素更廣泛地應(yīng)用于人畜醫(yī)療,作為一類新型內(nèi)分泌干擾物質(zhì),其直到近幾年才被人們關(guān)注,目前關(guān)于地表水中糖皮質(zhì)激素的檢測方法報道還非常少,對于其在環(huán)境中的遷移和毒理效應(yīng)一直受檢測手段的制約。因此建立靈敏、可靠的檢測方法是研究地理環(huán)境中糖皮質(zhì)激素環(huán)境污染及其生態(tài)效應(yīng)和風(fēng)險的前提條件和重要基礎(chǔ)。本文基于超高效液相色譜串聯(lián)質(zhì)譜技術(shù)結(jié)合固相萃取前處理方法建立了同時檢測地表水體中18種糖皮質(zhì)激素的高效方法；并針對北京部分水體,利用建立的檢測方法研究糖皮質(zhì)激素的環(huán)境污染水平和空間分布特征。配制18種糖皮質(zhì)激素的標(biāo)準(zhǔn)溶液,利用超高效液相色譜質(zhì)譜聯(lián)用儀,在多反應(yīng)選擇檢測模式(MRM)下,分別對糖皮質(zhì)激素檢測方法的正負(fù)離子模式、母離子、定量/定性離子、錐孔電壓、碰撞能量等相關(guān)質(zhì)譜采集參數(shù)和分離洗脫流動相程序進(jìn)行優(yōu)化,最終選擇ESI(-)模式,乙酸加合物作為母離子,甲醇/0.1%乙酸水溶液流動相等作為最終條件。通過考察標(biāo)樣添加回收率結(jié)果,優(yōu)化固相萃取前處理方法中的關(guān)鍵環(huán)節(jié),包括萃取柱、凈化柱和洗脫溶劑的選擇等。發(fā)現(xiàn)對于地表水樣,以親水親油平衡(HLB)柱為萃取柱,乙腈/乙酸乙酯(1：1,體積比)為洗脫溶劑就可以滿足分析要求,氨基柱等作為凈化柱并沒有顯示顯著的凈化效果。對檢測方法的考察結(jié)果表明：方法回收率在65～108%之間,相對標(biāo)準(zhǔn)偏差小于15%,方法檢出限除醋酸可的松和醋酸氫化可的松為10 ng/L外,其他物質(zhì)均在0.1～1.0 ng/L之間,該方法較為簡便、經(jīng)濟、高效,能滿足日常檢測的要求。利用建立的方法對北京清河中的糖皮質(zhì)激素污染狀況進(jìn)行研究,共檢出8種糖皮質(zhì)激素,濃度水平范圍為0.20 ng/L(地塞米松)～476 ng/L(醋酸氫化可的松),其中曲安西龍,曲安奈德,醋酸氫化可的松和丙酸氯倍他索是首次檢出；與國內(nèi)外糖皮質(zhì)激素污染狀況進(jìn)行比,發(fā)現(xiàn)調(diào)查水體中糖皮質(zhì)激素的污染處于相對嚴(yán)重的水平；分析其在清河水體中的空間分布特征,發(fā)現(xiàn)糖皮質(zhì)激素的濃度水平為：清河中游中上游下游；沿岸人口分布密度和土地利用類型是造成這種分布的主要原因。
[Abstract]:Endocrine disrupting substance (EDCs) has attracted the attention of researchers because it interferes with the normal function of endocrine system of organism at low concentration. Compared with estrogen, many kinds of glucocorticoids are widely used in human and animal medicine.As a new type of endocrine disrupting substance, it has not been paid much attention until recent years. At present, there are few reports on the detection of glucocorticoid in surface water.Its migration and toxicological effects in the environment are always restricted by the means of detection.Therefore, the establishment of a sensitive and reliable detection method is the precondition and important basis for studying the environmental pollution of glucocorticoid and its ecological effects and risks in geographical environment.In this paper, an efficient method for simultaneous detection of 18 kinds of glucocorticoids in surface water was established based on ultra-high performance liquid chromatography tandem mass spectrometry combined with solid phase extraction (SPE) pretreatment.The environmental pollution level and spatial distribution of glucocorticoids were studied by using the established detection method.18 standard solutions of glucocorticoids were prepared. The positive and negative ion mode, mother ion, quantitative and qualitative ion of glucocorticoid detection method were determined by super high performance liquid chromatography-mass spectrometer under multi-reaction selective detection mode (MRM).The parameters of mass spectrometry such as cone-hole voltage, collision energy and separation and elution mobile phase program were optimized. Finally, ESI-) mode was selected. Acetic acid adduct was used as the parent ion, and the flow of methanol / 0.1% acetic acid solution was equal as the final condition.By investigating the results of standard sample recovery, the key links of solid-phase extraction (SPE) pretreatment were optimized, including extraction column, purification column and elution solvent selection.It was found that for surface water samples, hydrophilic and lipophilic equilibrium (HLB) column was used as extraction column and acetonitrile / ethyl acetate (1: 1, volume ratio) as elution solvent.The results showed that the recovery rate of the method was between 65 and 108%, and the relative standard deviation was less than 15. The detection limit of the method was only 10 ng/L for cortisone acetate and 10 ng/L for hydrocortisone acetate. The method was simple and convenient.Economic, efficient, can meet the requirements of daily testing.Using the established method to study the status of glucocorticoid pollution in the Qinghe River in Beijing, 8 kinds of glucocorticoids were detected in the concentration range of 0.20 ng / L (dexamethasone, 476 ng / L) (hydrocortisone acetate, triamcinolone acetonide, triamcinolone acetonide, triamcinolone acetonide, triamcinolone acetonide, triamcinolone acetonide).Hydrocortisone acetate and clobetasol propionate were detected for the first time, and compared with the status of glucocorticoid pollution at home and abroad, it was found that the contamination of glucocorticoid in water was relatively serious.It was found that the concentration level of glucocorticoid was the middle and lower reaches of Qinghe River, and the distribution density and land use type of coastal population were the main reasons for the distribution of glucocorticoid.
【學(xué)位授予單位】：南京師范大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2015
【分類號】：X832

【參考文獻(xiàn)】

相關(guān)期刊論文 前4條

1 張豐松;李艷霞;黃澤春;楊明;;雌二醇在土壤/沉積物中的吸附特征及豬糞DOM對吸附的影響[J];環(huán)境科學(xué);2012年10期

2 孫俐;;酶聯(lián)免疫法測定動物源性食品中二苯乙烯類激素殘留量[J];食品研究與開發(fā);2008年06期

3 吳繼紅,張美莉,陳芳,廖小軍,胡小松;固相微萃取GC-MS法測定蘋果不同品種中主要芳香成分的研究[J];分析測試學(xué)報;2005年04期

4 孟娟,邵兵,吳國華,薛穎;氣相色譜-質(zhì)譜法同時測定動物性食品中8種β-興奮劑的殘留量[J];中國衛(wèi)生檢驗雜志;2005年06期

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