Determination of 11 Phthalate Esters in Beverages by Magnetic Solid-Phase Extraction Combined with High-Performance Liquid Chromatography. 2019

Shuo Yin, and Yi Yang, and Danni Yang, and Yongxin Li, and Yang Jiang, and Ling Wu, and Chengjun Sun
Sichuan University, West China School of Public Health, Chengdu 610041, China.

Background: Beverages can be easily contaminated by phthalate esters (PAEs) during the production, bottling, and transportation processes. It is necessary to determine the contamination level in beverages for assessment of human exposure. Objective: In this study, magnetic solid-phase extraction (MSPE) was combined with HPLC for the determination of 11 PAEs in beverages. Methods: Self-synthesized magnetic multiwalled carbon nanotubes (m-MWCNTs) were used as the adsorbent for PAE extraction. To extract the PAEs, an appropriate amount of m-MWCNTs and NaCl was added to the beverage sample. The mixture was mixed on a vortex mixer, the magnetic sorbent was collected with the aid of a magnet, and the supernatant was removed. Then, the analytes were eluted with n-hexane-acetone (1+1, v/v). Finally, the eluent was analyzed by the HPLC method. The separation was accomplished on a Phenomenex Luna-C18 column (250 × 4.6 mm, 5 μm), and the detection wavelength was set at 225 nm. Results: The linear ranges of the method were 2-300 μg/L with correlation coefficients greater than 0.9981. The LOD and LOQ were in the range of 0.659-5.33 × 10-2 μg/L and 2.20-17.8 × 10-2 μg/L, respectively. The recoveries of the method ranged from 79.8 to 114%, with the relative SDs less than 15.8%. The established method has been successfully applied for the determination of 11 PAEs in mineral water, carbonated soft drink, tea beverage, and fruit juice samples. PAEs were detected at 0.246-34.3 μg/L in these samples. Conclusions: The m-MWCNTs are the satisfactory sorbent for MSPE because of their strong adsorption capacity for PAEs. The established MSPE-HPLC method is rapid, easy, sensitive, green, and cost-effective. It can be applied to the analysis of trace PAEs in plastic bottled beverages. Highlights: Three magnetic nanoparticles (MNPs), including Fe₃O₄ MNPs, m-MWCNTs, and magnetic graphene oxide, were synthesized, and m-MWCNTs were chosen as the sorbent of MSPE for PAE extraction because of their strong adsorption capacity for PAEs. An MSPE-HPLC method has been developed for the analysis of 11 phthalates in plastic bottled beverages. The established method was successfully applied to the analysis of 11 phthalates in four types of beverage samples.

UI MeSH Term Description Entries
D010795 Phthalic Acids A group of compounds that has the general structure of a dicarboxylic acid-substituted benzene ring. The ortho-isomer is used in dye manufacture. (Dorland, 28th ed) Acids, Phthalic
D002253 Carbonated Beverages Drinkable liquids combined with or impregnated with CARBON DIOXIDE. Carbonated Drinks,Soda Pop,Soft Drinks,Beverage, Carbonated,Beverages, Carbonated,Carbonated Beverage,Carbonated Drink,Drink, Carbonated,Drink, Soft,Drinks, Carbonated,Drinks, Soft,Pop, Soda,Pops, Soda,Soda Pops,Soft Drink
D002851 Chromatography, High Pressure Liquid Liquid chromatographic techniques which feature high inlet pressures, high sensitivity, and high speed. Chromatography, High Performance Liquid,Chromatography, High Speed Liquid,Chromatography, Liquid, High Pressure,HPLC,High Performance Liquid Chromatography,High-Performance Liquid Chromatography,UPLC,Ultra Performance Liquid Chromatography,Chromatography, High-Performance Liquid,High-Performance Liquid Chromatographies,Liquid Chromatography, High-Performance
D004952 Esters Compounds derived from organic or inorganic acids in which at least one hydroxyl group is replaced by an –O-alkyl or another organic group. They can be represented by the structure formula RCOOR’ and are usually formed by the reaction between an acid and an alcohol with elimination of water. Ester
D005506 Food Contamination The presence in food of harmful, unpalatable, or otherwise objectionable foreign substances, e.g. chemicals, microorganisms or diluents, before, during, or after processing or storage. Food Adulteration,Adulteration, Food,Adulterations, Food,Contamination, Food,Contaminations, Food,Food Adulterations,Food Contaminations
D000067030 Fruit and Vegetable Juices The liquids extracted from plants. Fruit Juices,Vegetable Juices,Fruit Juice,Juice, Fruit,Juice, Vegetable,Juices, Fruit,Juices, Vegetable,Vegetable Juice
D000327 Adsorption The adhesion of gases, liquids, or dissolved solids onto a surface. It includes adsorptive phenomena of bacteria and viruses onto surfaces as well. ABSORPTION into the substance may follow but not necessarily. Adsorptions
D001628 Beverages Liquids that are suitable for drinking. (From Merriam Webster Collegiate Dictionary, 10th ed) Beverage
D013662 Tea The infusion of leaves of CAMELLIA SINENSIS (formerly Thea sinensis) as a beverage, the familiar Asian tea, which contains CATECHIN (especially epigallocatechin gallate) and CAFFEINE. Black Tea,Green Tea,Black Teas,Green Teas,Tea, Black,Tea, Green,Teas, Black,Teas, Green
D052616 Solid Phase Extraction An extraction method that separates analytes using a solid phase and a liquid phase. It is used for preparative sample cleanup before analysis by CHROMATOGRAPHY and other analytical methods. Extraction, Solid Phase,Extractions, Solid Phase,Solid Phase Extractions

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