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| Determination of Bisphenol Compounds in Drinking Water by High Performance Liquid Chromatography with Pipette Tip Solidphase Extraction Using Carboxylated Multiwalled Carbon Nanotubes as Adsorbent |
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| DOI： |
| KeyWord:carboxylated multi-walled carbon nanotubes bisphenol compounds high performance liquid chromatography drinking water solid-phase extraction |
| Author | Institution |
| ZHU Pei-jie，TU Xue-yuan，ZHOU Jia-huan，CHEN Yi-quan，LIU Yan-qing，WANG Hong-wu |
School of Food & Pharmaceutical Engineering， Zhaoqing University， Zhaoqing ， China |
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| 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. |
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