Dubey Monika, Vellanki Bhanu Prakash, Kazmi Absar Ahmad
Department of Civil Engineering, Indian Institute of Technology, Roorkee, Roorkee, Uttarakhand, India.
Anal Methods. 2020 Sep 17;12(35):4363-4376. doi: 10.1039/d0ay01131b.
Pharmaceuticals, personal care products, synthetic hormones, and industrial manufacturing additives are used worldwide, and their residues are frequently detected in wastewater. In this study, a sensitive and selective method was developed and validated for the detection and quantification of 14 Emerging Contaminants (ECs) with various physico-chemical properties frequently found in wastewater. Solid Phase Extraction (SPE) allowed for extraction and concentration of the compounds. Liquid chromatography-mass spectrometry in both positive and negative electrospray ionization mode was used for the analysis. Three different combinations of mobile phase, water + 0.1% formic acid : acetonitrile + 0.1% formic acid (3 compounds), water + 0.1% formic acid : methanol (5) and 10 mM ammonium acetate buffer : acetonitrile + 0.1% formic acid (6) gave the best chromatographic conditions to analyze the contaminants in real wastewater samples. Four different eluents at acidic and basic sample pH values were tested to optimize the SPE methodology, and three different dilution ratios (1 : 1, 2 : 1, and 5 : 1) were tested to reduce the matrix effect. Data validation was conducted using linearity, intra and inter-day repeatability, LOD/LOQ, percentage recovery, and percentage process efficiency studies. As a case study, a biological nutrient removal (BNR) based plant was tested for the presence of ECs using the developed method. Removal efficiency at different treatment stages was assessed. Most of the treatment occurred at the secondary treatment stage, whereas primary treatment and disinfection had little effect on removal. All the contaminants were found in the inlet wastewater. Estrone (E1), an endocrine disrupting compound, was reported for the first time in Indian wastewater at 376.2 ng L-1. Seven, four, and two ECs were removed at high, medium, and low efficiencies, respectively. Carbamazepine showed negative removal. This study enhanced our understanding of the occurrence and fate of several ECs in BNR based treatment systems.
药品、个人护理产品、合成激素和工业制造添加剂在全球范围内广泛使用，其残留物经常在废水中被检测到。在本研究中，开发并验证了一种灵敏且具选择性的方法，用于检测和定量废水中常见的14种具有不同物理化学性质的新兴污染物（ECs）。固相萃取（SPE）用于化合物的萃取和浓缩。采用正、负电喷雾电离模式的液相色谱-质谱联用进行分析。流动相的三种不同组合，即水 + 0.1%甲酸 : 乙腈 + 0.1%甲酸（3种化合物）、水 + 0.1%甲酸 : 甲醇（5种）和10 mM醋酸铵缓冲液 : 乙腈 + 0.1%甲酸（6种），给出了分析实际废水样品中污染物的最佳色谱条件。测试了酸性和碱性样品pH值下的四种不同洗脱液以优化SPE方法，并测试了三种不同稀释比（1 : 1、2 : 1和5 : 1）以降低基质效应。使用线性、日内和日间重复性、检测限/定量限、回收率百分比和处理效率百分比研究进行数据验证。作为案例研究，使用所开发的方法对基于生物营养物去除（BNR）的工厂进行了ECs检测。评估了不同处理阶段的去除效率。大部分处理发生在二级处理阶段，而一级处理和消毒对去除效果影响很小。所有污染物均在进水废水中被发现。雌激素（E1），一种内分泌干扰化合物，首次在印度废水中以376.2 ng L-1的浓度被报道。分别有七种、四种和两种ECs以高、中、低效率被去除。卡马西平呈现负去除率。本研究增进了我们对基于BNR的处理系统中几种ECs的存在情况和归宿的理解。
