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枪头式羧基化多壁碳纳米管固相萃取/高效液相色谱测定饮用水中双酚类化合物
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朱培杰,涂雪元,周家欢,陈奕全,刘艳清,汪洪武 肇庆学院 食品与制药工程学院广东 肇庆 526061 
基金项目:肇庆学院2018年自然科学青年项目(201816, 201817)
中文摘要:该文建立了一种枪头式羧基化多壁碳纳米管固相萃取/高效液相色谱检测饮用水中5种双酚类化合物的分析方法。系统考察了碳纳米管的种类和用量、样品溶液pH值、洗脱剂的种类和用量对方法回收率的影响。在最优实验条件下,双酚A(BPA)、双酚E(BPE)、双酚F(BPF)、双酚Z(BPZ)和四甲基双酚A(TMBPA)在2.2~220 μg/L范围内与其峰面积呈良好的线性关系(r ≥ 0.998 5),方法检出限(MDL)为0.005~0.097 μg/L。3个加标水平(22、110、220 μg/L)下,5种化合物的加标回收率为91.1%~110%,相对标准偏差(RSD)不大于4.3%。与文献报道的方法相比,该方法前处理简单、选择性好,检出限较低,可用于饮用水中双酚类化合物的快速定性与定量检测。
中文关键词:羧基化多壁碳纳米管  双酚类化合物  高效液相色谱  饮用水  固相萃取
 
Determination of Bisphenol Compounds in Drinking Water by High Performance Liquid Chromatography with Pipette Tip Solidphase Extraction Using Carboxylated Multiwalled Carbon Nanotubes as Adsorbent
Abstract:Bisphenol compounds are a type of environmental estrogens, which are mainly used in the synthesis of polycarbonate plastics, epoxy resins, polyester resins, etc. This type of estrogens often appear in different water environments such as tap water, rivers and lakes due to the incomplete polymerization in production process or the polymer degradation in use. Bisphenol compounds could cause great harm to human health and the survival of other organisms. Therefore, detection of bisphenol compounds in water is particularly important. In this study, a high performance liquid chromatography with pipette tip solid-phase extraction(PT-SPE) using carboxylated multi-walled carbon nanotubes as adsorbent was developed for the determination of 5 bisphenol compounds, i.e bisphenol A(BPA), bisphenol E(BPE), bisphenol F(BPF), bisphenol Z(BPZ) and tetramethyl bisphenol A(TMBPA) in drinking water. The water samples with different pH were adjusted by formic acid and ammonia solutions, then loaded into the PT-SPE cartridge. A Shim-pack GIST C18(250 mm × 4.6 mm, 5 μm) chromatographic column and an ultraviolet detector(UV) were used for the determination of bisphenol compounds. Effects of type and amount of the carbon nanotubes, pH value of the sample solution, and type and amount of the eluent on recovery of the method were systematically investigated in this paper. The experimental results showed that the enrichment effect of carboxylated multi-carbon nanotubes was significantly better than those of aminated multi-walled carbon nanotubes and hydroxylated multi-walled carbon nanotubes. With the increase of dosage of carboxyl multi-walled carbon nanotubes from 0.5 mg to 2.0 mg, the recoveries for five bisphenol compounds increased firstly and then decreased. When the dosage reached 1.5 mg, the highest recoveries were obtained. The pH values of water samples were also one of the important factors affecting the adsorption of bisphenol compounds by multi-walled carbon nanotubes. When the pH values varied from 3 to 5, the recoveries increased slightly, and the highest recovery was obtained at pH 5. As the pH values continued to increase(pH 5-7), the recoveries showed a downward trend. The type and amount of eluent could also affect the recoveries and enrichment of bisphenol compounds in solid-phase extraction. After systematical optimization, 0.5 mL methanol was finally selected as the eluent. Under the optimal experimental conditions, good linear relationships for 5 bisphenol compounds were obtained in the range of 2.2-220 μg/L with correlation coefficients(r) not less than 0.998 5. Method detection limits(MDL) of the developed method were in the range of 0.005-0.097 μg/L. The recoveries for the bisphenol compounds at three spiked levels of 22, 110, 220 μg/L ranged from 91.1% to 110%, with relative standard deviations(RSD) not more than 4.3%. Compared with previous reported methods, this method exhibited several advantages such as simple pretreatment, good selectivity and low detection limit, which could be used for the determination of bisphenol compounds in drinking water.
Key Words:carboxylated multi-walled carbon nanotubes  bisphenol compounds  high performance liquid chromatography  drinking water  solid-phase extraction
引用本文:朱培杰,涂雪元,周家欢,陈奕全,刘艳清,汪洪武.枪头式羧基化多壁碳纳米管固相萃取/高效液相色谱测定饮用水中双酚类化合物[J].分析测试学报,2021,40(9):1328-1333.
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