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液相色譜—質(zhì)譜聯(lián)用法檢測北京市飲用水中雙酚A

發(fā)布時間:2018-01-19 08:44

  本文關(guān)鍵詞: 飲用水 雙酚A 液相色譜-質(zhì)譜法 檢測 固相萃取 出處:《首都經(jīng)濟貿(mào)易大學》2017年碩士論文 論文類型:學位論文


【摘要】:雙酚A(Bisphenol A,BPA)常被用來合成高分子材料,其制品廣泛存在于日常生活中,并隨著人們對它的使用而在環(huán)境中遷移擴散。然而,BPA是一種對人體有害的環(huán)境內(nèi)分泌干擾物(Environmental Endocrine Disruptors,EEDs),我國《生活飲用水衛(wèi)生標準》(GB 5749-2006)中規(guī)定其限值為0.01 mg/L。本研究首先建立固相萃取-液相色譜-質(zhì)譜聯(lián)用法檢測飲用水中的BPA,對樣品前處理條件和儀器檢測條件進行優(yōu)化,并對所建立的方法進行評價。進而,運用該方法檢測北京市自來水、桶裝水和瓶裝水中的BPA,調(diào)查北京市飲用水中BPA的污染情況,分析BPA的來源,為BPA的人體膳食暴露評估提供科學依據(jù)。主要的結(jié)果如下:經(jīng)優(yōu)化的樣品前處理條件為:C18固相萃取柱,上樣流速1~2 m L/min,洗脫液為9m L甲醇。經(jīng)優(yōu)化的儀器檢測條件為:色譜柱為ZORBAX Extend-C18柱(4.6×150 mm,5μm);流動相為甲醇-水(95:5,V/V),流速為1.0 mL/min;干燥氣流速為11 L/min,干燥氣溫度為350℃,霧化氣壓力為35 psi。在此條件下,樣品峰和雜質(zhì)峰的分離度好,峰形對稱,滿足檢測要求。用超純水配制質(zhì)量濃度范圍為122.9~1190.7 ng/L的水樣,經(jīng)樣品前處理后上機檢測,建立一級質(zhì)譜峰面積-濃度標準曲線,線性回歸方程y=69.4x+2186.1,相關(guān)系數(shù)為0.9929。方法的檢出限為7.0 ng/L,定量限為23.5 ng/L。方法的回收率為78.8~108.1%,相對標準偏差(n=6)≤13.5%。該方法選擇性好、靈敏度高、重現(xiàn)性好,能夠滿足定量檢測飲用水中BPA的要求。56種包裝飲用水中有36種檢出BPA,檢出率為64.3%;8個城區(qū)的24個自來水樣中有3個檢出BPA,檢出率為12.5%,最高檢出濃度為1592.8 ng/L。BPA主要來自飲用水水體、包裝材料、運輸材料、飲水設(shè)備、飲水器皿五個方面。北京市飲用水中尤其是桶裝飲用水中較為普遍地存在BPA,長期飲用有健康風險。
[Abstract]:Bisphenol A bisphenol BPA is often used to synthesize polymer materials. Its products are widely used in daily life and migrate in the environment with the use of bisphenol A. However. BPA is an environmental endocrine disruptor that is harmful to human body. The hygienic Standard of drinking Water in China (GB5749-2006). In this study, a solid-phase extraction-liquid chromatography-mass spectrometry method was established for the detection of BPA in drinking water. The conditions of sample pretreatment and instrument detection were optimized, and the established method was evaluated. Furthermore, the BPA in tap water, bottled water and bottled water in Beijing was detected by this method. The pollution of BPA in drinking water in Beijing was investigated and the source of BPA was analyzed. The main results were as follows: the optimized sample pretreatment condition was: the sample was extracted by solid phase extraction column with a flow rate of 1 ~ 2 mL 路min ~ (-1) m ~ (-1) 路min ~ (-1) 路m ~ (-1) 路min ~ (-1) 路L ~ (-1) ~ (-1). The elution solution was 9ml methanol. The optimized instrument conditions were as follows: the chromatographic column was ZORBAX Extend-C18 column (4.6 脳 150mm ~ 5 渭 m); The mobile phase consisted of methanol-water 95: 5 V / V, and the flow rate was 1.0 mL / min. The drying gas flow velocity is 11 L / min, the drying gas temperature is 350 鈩,

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