scholarly journals Application of a Liquid-Liquid Microextraction Method Based on a Natural Hydrophobic Deep Eutectic Solvent for the Extraction of Plastic Migrants from Kombuchas

Molecules ◽  
2021 ◽  
Vol 27 (1) ◽  
pp. 178
Author(s):  
Antonio Herrera-Herrera ◽  
Ruth Rodríguez-Ramos ◽  
Álvaro Santana-Mayor ◽  
Bárbara Socas-Rodríguez ◽  
Miguel Rodríguez-Delgado
Keyword(s):  
High Performance ◽  
Dibutyl Phthalate ◽  
Phthalate Esters ◽  
Deep Eutectic Solvent ◽  
Quadrupole Mass ◽  
Limit Of Quantification ◽  
Limits Of Detection ◽  
Fermented Beverage ◽  
Plastic Containers ◽  
Liquid Microextraction

A vortex-assisted liquid-liquid microextraction, based on a natural hydrophobic deep eutectic solvent made from the monoterpene thymol and octanoic fatty acid, was employed for the analysis of 11 phthalate esters and one adipate in kombucha (a tea-based fermented beverage). Separation and determination were performed using an ultra-high performance liquid chromatography (UHPLC) system coupled to a single quadrupole mass spectrometer. Confirmatory analyses were carried out through UHPLC tandem mass spectrometry. The full method was validated in terms of matrix effect, matrix-matched calibration, sensitivity, recovery, limits of detection and quantification and repeatability. Satisfactory determination coefficients for quadratic calibration curves (≥0.9938), recovery values (67–120%) and limits of detection (0.07–5.45 µg/L) were obtained. Analysis of 26 kombucha samples reported concentrations for dibutyl phthalate and dimethyl phthalate in the range between the limit of quantification (LOQ) and 16.18 ± 1.14 µg/L, although these phthalates were also detected under the LOQ in some of the analyzed samples. Only one of the samples bottled in plastic containers (7) did not present residues while only five of the 19 samples in glass bottles contained any plasticizer. However, the highest concentration was found in a kombucha bottled in food-grade glass. This work represents the first application in which phthalates and adipates are analyzed in kombuchas.

Determination of Selected Phthalates in Some Commercial Cosmetic Products by HPLC-UV

2020 ◽  
Vol 23 (10) ◽  
pp. 1010-1022
Author(s):  
Emrah Dural
Keyword(s):  
High Performance ◽  
Phthalate Esters ◽  
High Sensitivity ◽  
Hplc Method ◽  
Cosmetic Products ◽  
Limit Of Quantification ◽  
Nail Polish ◽  
Accuracy And Precision ◽  
Butyl Phthalate

Aim and scope: Due to the serious toxicological risks and their widespread use, quantitative determination of phthalates in cosmetic products have importance for public health. The aim of this study was to develop a validated simple, rapid and reliable high-performance liquid chromatography (HPLC) method for the determination of phthalates which are; dimethyl phthalate (DMP), diethyl phthalate (DEP), benzyl butyl phthalate (BBP), di-n-butyl phthalate (DBP), di(2- ethylhexyl) phthalate (DEHP), in cosmetic products and to investigate these phthalate (PHT) levels in 48 cosmetic products marketing in Sivas, Turkey. Materials and Methods: Separation was achieved by a reverse-phase ACE-5 C18 column (4.6 x 250 mm, 5.0 μm). As the mobile phase, 5 mM KH2PO4 and acetonitrile were used gradiently at 1.5 ml min-1. All PHT esters were detected at 230 nm and the run time was taking 21 minutes. Results: This method showed the high sensitivity value the limit of quantification (LOQ) values for which are below 0.64 μg mL-1 of all phthalates. Method linearity was ≥0.999 (r2). Accuracy and precision values of all phthalates were calculated between (-6.5) and 6.6 (RE%) and ≤6.2 (RSD%), respectively. Average recovery was between 94.8% and 99.6%. Forty-eight samples used for both babies and adults were successfully analyzed by the developed method. Results have shown that, DMP (340.7 μg mL-1 ±323.7), DEP (1852.1 μg mL-1 ± 2192.0), and DBP (691.3 μg mL-1 ± 1378.5) were used highly in nail polish, fragrance and cream products, respectively. Conclusion: Phthalate esters, which are mostly detected in the content of fragrance, cream and nail polish products and our research in general, are DEP (1852.1 μg mL-1 ± 2192.0), DBP (691.3 μg mL-1 ± 1378.5) and DMP (340.7 μg mL-1 ±323.7), respectively. Phthalates were found in the content of all 48 cosmetic products examined, and the most detected phthalates in general average were DEP (581.7 μg mL-1 + 1405.2) with a rate of 79.2%. The unexpectedly high phthalate content in the examined cosmetic products revealed a great risk of these products on human health. The developed method is a simple, sensitive, reliable and economical alternative for the determination of phthalates in the content of cosmetic products, it can be used to identify phthalate esters in different products after some modifications.

Supramolecular Solvent Based Liquid-Liquid Microextraction for Preconcentration of Selected Fluoroquinolone Antibiotics in Environmental Water Sample Prior to High Performance Liquid Chromatographic Determination

2019 ◽  
Vol 15 (6) ◽  
pp. 607-615 ◽  
Author(s):  
Shirley K. Selahle ◽  
Philiswa N. Nomngongo
Keyword(s):  
High Performance ◽  
Chromatographic Determination ◽  
Decanoic Acid ◽  
Environmental Water ◽  
High Performance Liquid Chromatographic ◽  
Array Detector ◽  
Optimum Conditions ◽  
Limit Of Quantification ◽  
Supramolecular Solvent ◽  
Liquid Microextraction

Background and Objective: A rapid, simple and environmental friendly supramolecular solvent (SUPRAS) based liquid-liquid microextraction method for preconcentration of ciprofloxacin (CIPRO), danofloxacin (DANO) and enrofloxacin (ENRO) from wastewater was developed. Methods: This microextraction technique was coupled with high-performance liquid chromatography equipped with a diode array detector (HPLC-PDA) for detection and separation of the antibiotics. The SUPRAS composed of decanoic acid and tricaprylymethylammonium chloride. Optimum conditions for the extraction and preconcentration of all the antibiotics were obtained using surface response methodology (RSM) based on Box-Behnken design. Results: Under optimum conditions, the limits of detection (LOD) and limit of quantification (LOQ) ranged from 0.06-0.14 µg L−1 and 0.22-0.47 μg L−1, respectively with the preconcentration factors ranging from 153-241. The linear dynamic ranges were between LOQ and 850 µg L−1 with correlation coefficients ranging from 0.9928 to 0.9999. The intra-day (n = 15) and inter-day (n = 5) precisions (expressed in terms of %RSD) for 50 µg L−1 of CIPRO, DANO and ENRO were in the range of 3.3–4% and 4.1–5.8%, respectively. Conclusion: Lastly, the developed method was used for the extraction, preconcentration and quantification of selected CIPRO, DANO and ENRO in influent and effluent wastewater samples.

An Effective Acid–Base-Induced Liquid–Liquid Microextraction Based on Deep Eutectic Solvents for Determination of Testosterone and Methyltestosterone in Milk

2020 ◽  
Vol 58 (9) ◽  
pp. 880-886
Author(s):  
Xiao Li ◽  
Tao Yuan ◽  
Ting Zhao ◽  
Xiaomei Wu ◽  
Yaling Yang
Keyword(s):  
Hydrogen Bond ◽  
Hydrochloric Acid ◽  
High Performance ◽  
Deep Eutectic Solvent ◽  
Deep Eutectic Solvents ◽  
Hydrogen Bond Donor ◽  
Acid Base ◽  
Hydrogen Bond Acceptor ◽  
Liquid Microextraction

Abstract An environmentally friendly method for the determination of testosterone and methyltestosterone by acid–base-induced deep eutectic solvents liquid–liquid microextraction (DES-ABLLME) combining with high-performance liquid chromatography was established. The deep eutectic solvent (DES) consisting of menthol:lauric acid:decanoic acid (3:1:1) can act as both hydrogen bond donor and hydrogen bond acceptor. In this approach, ammonia solution (NH3•H2O) is used as an emulsifier to react with DESs in the extraction process to generate salt and form milky white solution, achieving high extraction efficiency. Hydrochloric acid was used as a phase separator to change the emulsification state and promote the separation of extraction agent from water phase. A series of parameters were optimized including the volume of DES and the emulsifying agent, glucose concentration as well as hydrochloric acid volume. The method was linear in the range 0.5–100 μg mL−1 with a correlation coefficient (R) of 0.9999, and the limits of detection were 0.067 and 0.2 μg mL−1 for testosterone and methyltestosterone, respectively. This method was applied to analyze testosterone and methyltestosterone in milk samples, and the recoveries were between 89.2 and 108.2%.

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