液相色谱—质谱联用法检测北京市饮用水中双酚A

发布时间：2018-01-19 08:44

  本文关键词： 饮用水 双酚A 液相色谱-质谱法 检测 固相萃取　出处：《首都经济贸易大学》2017年硕士论文　论文类型：学位论文

【摘要】：双酚A(Bisphenol A,BPA)常被用来合成高分子材料,其制品广泛存在于日常生活中,并随着人们对它的使用而在环境中迁移扩散。然而,BPA是一种对人体有害的环境内分泌干扰物(Environmental Endocrine Disruptors,EEDs),我国《生活饮用水卫生标准》(GB 5749-2006)中规定其限值为0.01 mg/L。本研究首先建立固相萃取-液相色谱-质谱联用法检测饮用水中的BPA,对样品前处理条件和仪器检测条件进行优化,并对所建立的方法进行评价。进而,运用该方法检测北京市自来水、桶装水和瓶装水中的BPA,调查北京市饮用水中BPA的污染情况,分析BPA的来源,为BPA的人体膳食暴露评估提供科学依据。主要的结果如下:经优化的样品前处理条件为:C18固相萃取柱,上样流速1~2 m L/min,洗脱液为9m L甲醇。经优化的仪器检测条件为:色谱柱为ZORBAX Extend-C18柱(4.6×150 mm,5μm);流动相为甲醇-水(95:5,V/V),流速为1.0 mL/min;干燥气流速为11 L/min,干燥气温度为350℃,雾化气压力为35 psi。在此条件下,样品峰和杂质峰的分离度好,峰形对称,满足检测要求。用超纯水配制质量浓度范围为122.9~1190.7 ng/L的水样,经样品前处理后上机检测,建立一级质谱峰面积-浓度标准曲线,线性回归方程y=69.4x+2186.1,相关系数为0.9929。方法的检出限为7.0 ng/L,定量限为23.5 ng/L。方法的回收率为78.8~108.1%,相对标准偏差(n=6)≤13.5%。该方法选择性好、灵敏度高、重现性好,能够满足定量检测饮用水中BPA的要求。56种包装饮用水中有36种检出BPA,检出率为64.3%;8个城区的24个自来水样中有3个检出BPA,检出率为12.5%,最高检出浓度为1592.8 ng/L。BPA主要来自饮用水水体、包装材料、运输材料、饮水设备、饮水器皿五个方面。北京市饮用水中尤其是桶装饮用水中较为普遍地存在BPA,长期饮用有健康风险。
[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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