Method For Determination Of Bisphenol Research Articles

Development of a new method for determination of bisphenol A based on stirrer-assisted switchable hydrophilic solvent-based liquid phase microextraction coupled with electrochemical sensor

In this work, a novel stirrer-assisted liquid-phase microextraction method using switchable hydrophilic solvents was developed for the extraction and preconcentration of bisphenol A from real samples prior to electrochemical analysis. For the first time, the effect of stirring while switching the extraction solvent (N,N-dipropylamine, DPA) was investigated, and the use of stirring instead of temperature change, which is a time-consuming process, hazardous acids (e.g., HCl), and dry ice was used for bisphenol A extraction based on switchable solvents. Various parameters such as solvent type, solvent volume, stirring time, and stirring speed were optimized. The optimized conditions were 100 μl DPA, 2 min extraction time, 30 s stirring time, 700 rpm stirring speed, and solution pH of 7.0. A theoretical study was also conducted to show the effects of stirring on the homogenization of the phases. The proposed method offers some advantages, such as simplicity, use of a small amount of inexpensive and less hazardous reagents, rapid extraction, and shorter analysis time. Under the optimized conditions for the developed method, LOQ and LOD were obtained to be 0.01 and 0.003 μM, respectively. Moreover, the calibration curves were linear in the range of 0.01–250 μM. The proposed method was used for the determination of bisphenol A in food and water samples.

Validated GC–MS method for determination of bisphenol a and its five analogues in dietary and nutritional supplements

Bisphenol A (BPA) and its analogues showing structural and functional similarity to BPA are commonly applied in various industrial applications and thus are becoming ubiquitous in the environment. At the same time there is increasing scientific evidence that exposure to these chemicals may lead to adverse health effects in human and wildlife. In recent years dietary and nutritional supplements dedicated for athletes have become more popular and are widely used even by people who are not professionals. This study presents the development, optimization and validation of an analytical procedure for determination of six bisphenol analogues in dietary supplements using gas chromatography – mass spectrometry technique. All validation parameters met the established acceptance criteria in accordance with international guidelines. The method was linear within the tested range of 50–1000 ng/mL, the limit of quantitation was set as the lowest calibration point 50 ng/mL, detection limit for each bisphenol was calculated as standard estimation error on the basis of the linearity testing and was in the range of 8.73–15.44 ng/mL. Method trueness, accuracy (within and between runs) and precision were also verified and were in the range of 78.8 – 100.4%, 94.3 – 103.1%,0.5 – 9.6% respectively.The developed procedure was successfully applied for real samples analysis, namely for fifteen sport supplements of different composition and designated for various purposes, i.e. for increasing effectiveness, promoting muscle recovery and endurance, reducing tiredness and fatigue or increasing immune ability. For the majority of samples, bisphenols were either not detected or detected at the LOD level except bisphenol A which was quantitated in few samples at LOQ level or higher (in the range 0.852–2.892 ng/mg)The field of bisphenol analogues analytics has increased in recent years due to law regulations becoming more strict, thus the development of new analytical tools for quality control of dietary products is needed and fully justified.

Validated Gc-Ms Method for Determination of Bisphenol a and its Five Analogues in Dietary and Nutritional Supplements

Validated Gc-Ms Method for Determination of Bisphenol a and its Five Analogues in Dietary and Nutritional Supplements

Molecularly Imprinted Polymer-Coated Vial Solid-Phase Microextraction as a Selective and Manual Method for Determination of Bisphenol a in Mineral and River Water Samples

In this work, we introduce the novel solid-phase microextraction methods using molecularly imprinted polymer-coated to the inner surface of a commercial 10 mL serum vial. In this method that named with molecularly imprinted polymer-coated vial solid-phase microextraction (MIP-CV-SPME), the fabricated vials obtained through thermal-polymerization on the surface of silylated vials to achieve a chemically bonded coating bisphenol A imprinted polymer. A 1 mL of sample solution was added to the fabricate vial and after simple and rapid manual extraction and elution process, the target compound was injected into HPLC for analysis. The essential factors that influenced the extraction efficiency such as type and volume of elution solvent, extraction time, pH, and ionic strength of sample were optimized and in optimum values, the repeatability for one device was 2.2%. The detection limits for the studied compound was 0.006 µgL−1. The method does not need any particular apparatus and commercially can be used in common laboratories.

A fast and direct determination of bisphenol S in thermal paper samples using paper spray ionization mass spectrometry.

Concerns about human health regarding the large use of bisphenol A in thermal papers have led to its replacement by bisphenol S. Analyses of bisphenols require several sample pretreatment steps, which are laborious, expensive, and time-consuming. A paper spray ionization mass spectrometry (PSI-MS) was developed to detect and quantify bisphenol S in three different brands of thermal papers commercially available. Parameters such as paper size, and paper position relative to the mass spectrometer inlet were evaluated. The analyses were performed in selected ion monitoring mode on a linear ion trap mass spectrometer. The developed method presented absolute recovery values ranging from 92.2 to 109.04%, accuracy values from -1.2 to 9.0%, and inter assay precision from 1.8 to 5.6% and enabled LOD as low as 5 ng g-1. The concentration of bisphenol S in all of the three brands of BPA-free thermal papers evaluated ranged from 1.36 to 6.77 μg g-1, and the concentrarion of BPA ranged from 6.56 to 16.4 μg g-1 in all samples of thermal paper evaluated. The PSI-MS method described here was comparable to the conventional ones, such as liquid chromatography coupled with mass spectrometry and gas chromatography coupled with mass spectrometry described in the literature. The present study proved to be practical, fast, and efficient for the direct determination of bisphenol S in thermal papers. Furthermore, the methodology here described showed to be a promising alternative to replace the classical methods for determination of bisphenol S, due to its simplicity, and no needing of any sample pretreatment.

High-performance liquid chromatography (HPLC)-fluorescence method for determination of bisphenol A diglycidyl ether (BADGE) and its derivatives in canned foods

Bisphenol A diglycidyl ether (BADGE) is used as a raw material for the production of epoxy resins and PVC organosols, which are commonly applied as inner coatings for food cans. BADGE and its derivatives can migrate from coatings to foodstuffs during processing and storage thereby creating adverse health issues. In this work, a method based on high-performance liquid chromatography (HPLC)-fluorescence detection (FLD) method was developed for the rapid determination of BADGE and its five derivatives in canned foods. Modeling software DryLab® was applied for the optimization of separation conditions. An adequate separation was achieved in 5 min including equilibration time, using a core–shell particle column; such application has not been reported so far. Also, the results showed that LOD varied from 0.01 to 0.20 ng/g, while LOQ varied from 0.03 to 0.66 ng/g, and RSD was found to be <8.64%. The analytical recoveries ranged from 70.46 to 103.44%. Excellent validation data revealed that this method is suitable for the investigation of can coating-to-food migration of BADGE and its derivatives. The HPLC-FLD method is rapid, inexpensive and highly efficient, which could be applicable for safety inspection of food contact materials involving BADGE and its derivatives.

QbD-driven development and validation of HPLC method for determination of Bisphenol A and Bis-sulphone in environmental samples

ABSTRACTA large number of hazardous chemicals have entered the environment due to the rapid growth of urbanisation and industrial development and are exerting harmful effects on wildlife as well as on human health. Plastic materials are one of the most leading causes for this contamination which are widely used in daily activities of human beings, i.e. disposal purpose, food packaging, bottles, containers, cups, grocery bags, etc. These materials contain Bisphenol A (BPA) and Bis-sulphone (BIS) which have been recognised as potential endocrine disruptors. In the present study, a selective and reliable high-performance liquid chromatography (HPLC) based method was developed with the mobile phase of 10 mM ammonium acetate buffer-acetonitrile (58:42 v/v, pH: 5) using quality by design (QbD) approach and the method was validated for the simultaneous assessment of BPA and BIS. The method was observed with a good linearity range of 50–500 ng/mL with an r2 value of 0.998 and 0.999 for BPA and BIS, respectively. The developed and validated method was applied for the estimation of endocrine-disrupting chemicals in sewage water and soil samples. The results showed a considerable amount of BPA and BIS in the samples. This preliminary data explored the presence of BPA and BIS in these environmental samples that give the primary awareness of the effluence of BPA and BIS in the environment.

Determination of four parabens and bisphenols A, F and S in human breast milk using QuEChERS and liquid chromatography coupled to mass spectrometry

For the first time, a multiresidue, sensitive and high throughput method for determination of bisphenol A, F and S and 4 parabens (methyl paraben, ethyl paraben, propyl paraben and butyl paraben) in human breast milk was developed. The proposed method includes an extraction and clean-up procedure based on QuEChERS methodology followed by liquid chromatography coupled to triple quadrupole mass spectrometry determination. Negative atmospheric pressure chemical ionization in the selected reaction monitoring mode was used for mass detection. During the method validation the recoveries varied between 83 and 115% with a precision lower than 20% for all analytes using spiked levels from 0.1 to 50 ng mL−1. The LOQ was 0.10 ng mL−1 for most of the analytes. The proposed method was successfully applied for the determination of these compounds in 10 breast milk samples from volunteer lactating mothers from the Valencian region (Spain). Among parabens, methyl paraben presented the highest detection frequency (80%) with a concentration range of 0.11–7.00 ng mL−1, while bisphenol A was detected more frequently than BPF and BPS (80% of detection frequency) with concentrations ranging from 0.13 to 1.62 ng mL−1.

Detection of Bisphenol A in Water Samples by Magnetic Graphene Oxide Based Solid Phase Extraction and Liquid Chromatography

Bisphenol A (BPA) has received much attention from the public due to its endocrine disrupting effect. Therefore it is necessary to develop suitable analytical methods for determination of bisphenol A in water samples. In this study, magnetic graphene oxide was prepared and used as the sorbent for magnetic solid phase extraction of bisphenol A from aqueous solutions. The parameters which influence the extraction efficiency of bisphenol A were investigated. The optimum conditions, such as sample pH, extraction and desorption times, and eluent type and volume were obtained. The analytical performance of the method was evaluated, and the results showed that the limit of detection (LOD) for bisphenol A was 0.36μg/L and the RSD was 2.9 %. The developed method was applied to the detection of bisphenol A in environmental water samples with satisfactory recoveries.

Analytical methods for determination of bisphenol A, 4-tert-octylphenol and 4-nonylphenol in herrings and physiological fluids of the grey seal

•The aim of this work was to develop the methods of determination for phenol derivatives: bisphenol A (BPA), 4-tert-octylphenol (OP) and 4-nonylphenol (NP), in the whole body of herring Clupea harengus and in physiological fluids of the Baltic grey seal Halichoerus grypus grypus (blood and milk).•Methods were based on liquid chromatography coupled with a fluorescence detector (HPLC-FL).•These methods were satisfactorily validated, each showing good recovery (>80%) and precision (RSD?<?15%). Regarding the limit of quantification (LOQ), this was established at <2 ng?g-1 for herring, <0.07 ng?cm-3 for blood and <0.1 ng?cm-3 for milk.

Determination of Phenolic Endocrine Disruptors in Cosmetics by High-Performance Liquid Chromatography Mass Spectrometry

ABSTRACTAn analytical method for the simultaneous determination of bisphenol A, 4-t-octylphenol, 4-n-octylphenol, and 4-n-nonylphenol in cosmetic samples has been developed. These compounds have toxic effects on human health as they have shown to produce endocrine disrupting properties. Therefore, their presence in cosmetics should be avoided according to the current European Regulations on cosmetic products. The method is based on high-performance liquid chromatography coupled to mass spectrometry (HPLC-MS) detection. Standard addition calibration was used to avoid matrix effects. The limits of detection values ranged between 7 and 15 ng mL−1 (threefold of the residual standard deviation of regression lines). The proposed method was validated, and good recovery (90–106%) and repeatability values (2.7–8.2%) were obtained. Finally, the method was successfully applied to ten commercially available cosmetic samples. The good analytical features of the proposed method make it useful to carry out the quality control of cosmetic products and raw materials to assure the safety of users.

Colorimetric method for determination of bisphenol A based on aptamer-mediated aggregation of positively charged gold nanoparticles

A sensitive, specific and rapid colorimetric aptasensor for the determination of the plasticizer bisphenol A (BPA) was developed. It is based on the use of gold nanoparticles (AuNPs) that are positively charged due to the modification with cysteamine which is cationic at near-neutral pH values. If aptamers are added to such AuNPs, aggregation occurs due to electrostatic interactions between the negatively-charged aptamers and the positively-charged AuNPs. This results in a color change of the AuNPs from red to blue. If a sample containing BPA is added to the anti-BPA aptamers, the anti-BPA aptamers undergo folding via an induced-fit binding mechanism. This is accompanied by a conformational change, which prevents the aptamer-induced aggregation and color change of AuNPs. The effect was exploited to design a colorimetric assay for BPA. Under optimum conditions, the absorbance ratio of A527/A680 is linearly proportional to the BPA concentration in the range from 35 to 140 ng∙mL−1, with a detection limit of 0.11 ng∙mL−1. The method has been successfully applied to the determination of BPA in spiked tap water and gave recoveries between 91 and 106 %. Data were in full accordance with results obtained from HPLC. This assay is selective, easily performed, and in our perception represents a promising alternative to existing methods for rapid quantification of BPA.

Determination of Bisphenol A in Receipts and Carbon Paper by HPLC-UV

A simple and efficient method for determination of Bisphenol A (BPA), an endocrine disrupting chemical (EDC), is developed without the requirement of derivatization. Due to the prevalence of exposure of BPA-containing products to the general public, high-quality testing and monitoring methods are essential. BPA was separated and quantified under reverse-phase conditions using a high-performance liquid chromatography/ultraviolet absorption (HPLC-UV) detection method. A silica hydride-based C8 column along with an effective gradient protocol yielded well-resolved peaks that allowed for the direct analyses of BPA in receipt paper and carbon copies of lab notebooks. Excellent linear correlation was observed (R2 = 0.9936) in the calibration curve obtained from the HPLC-UV analyses.

A novel chemiluminescence method for determination of bisphenol Abased on the carbon dot-enhanced [formula omitted]–H2O2 system

A simple and sensitive chemiluminescence (CL) method on the basis of carbon dot (C-dot) enhanced HCO3−–H2O2 system, is designed for the determination of bisphenol A (BPA). The very weak CL of the HCO3−–H2O2 system is enhanced by a factor of ~100 in the presence of C-dots. Possible mechanisms that lead to the effect were elucidated by recording fluorescence and CL spectra and studying the effect of some radical scavengers. This enhancement is inhibited by BPA in the concentration range from 1.0 to 100µgL−1. This is exploited for its trace determination with a detection limit (3s) of 0.3µgL−1. The established method was applied to the determination of BPA in baby bottle and water samples with satisfactory results.

Development of HPLC-MS/MS method for the simultaneous determination of environmental phenols in human urine

We present a sensitive method for simultaneous determination of bisphenol A (BPA), benzophenone-3 (BP-3), 4-tert-octylphenol (t-OP), ortho-phenylphenol (OPP), four parabens (methyl, ethyl, propyl, butyl parabens) and five chlorophenols (2,4-dichlorophenol (2,4-DCP), 2,5-dichlorophenol (2,5-DCP), 2,4,5-trichlorophenol (2,4,5-triclorophenol), 2,4,6-trichlorophenol (2,4,6-TCP), and triclosan (TCS)), in human urine by high-pressure liquid chromatography (HPLC) mass spectrometry (MS). Samples were processed using enzymatic deconjugation of glucuronides followed by solid phase extraction (SPE) on a C18 cartridge and the eluate was concentrated. Analytes were separated by reversed-phase HPLC and then detected by atmospheric pressure chemical ionisation (APCI) MS and quantified by isotope dilution method. We describe details for optimisation of each step of the procedure. The sample treatment steps are straightforward and not labour-intensive and, therefore, permit a high sample throughput with excellent prospects for automation. This method shows low inter-day variation, and detection limits for most of the compounds are below 1 ng/mL in 1 mL of urine. The method accuracy was also verified by the analysis of proficiency testing urine samples.

Voltammetric determination of bisphenol A in food package by a glassy carbon electrode modified with carboxylated multi-walled carbon nanotubes

A highly sensitive and mercury-free method for determination of bisphenol A (BPA) was established using a glassy carbon electrode that was modified with carboxylated multi-walled carbon nanotubes. A sensitive oxidation peak is found at 550 mV in linear sweep voltammograms at pH 7. Based on this finding, trace levels of bisphenol A can be determined over a concentration range that is linear from 10 nM to 104 nM, the correlation coefficient being 0.9983, and the detection limit (S/N = 3) being 5.0 nM. The method was successfully applied to the determination of BPA in food package.

Amperometric determination of bisphenol A in milk using PAMAM–Fe 3O 4 modified glassy carbon electrode

A simply and sensitively electroanalytical method for determination of bisphenol A (BPA) using poly(amidoamine) (PAMAM) and Fe 3O 4 magnetic nanoparticles modified glassy carbon electrode (GCE) was presented. Compared with bare electrode, PAMAM–Fe 3O 4 modified electrode not only significantly enhanced the oxidation peak current of BPA, but also lowered the oxidation overpotential, suggesting that the modified electrode can remarkably improve the determining sensitivity of BPA. Factors influencing the detection processes were optimised and kinetic parameters were calculated. Under the optimal conditions, the oxidation current increased linearly with increasing the concentration of BPA in the range of 1 × 10 −8–3.07 × 10 −6 M with the correlation coefficient of 0.9996 and the detection limit of 5 × 10 −9 M. The current reached 95% of the steady-state current within about 6 s. The proposed method was successfully applied to determine BPA in milk samples and satisfactory results were obtained.

Dispersive liquid–liquid microextraction based on ionic liquid in combination with high-performance liquid chromatography for the determination of bisphenol A in water

A method termed dispersive liquid–liquid microextraction (DLLME) coupled with high-performance liquid chromatography-variable wavelength detection (HPLC-VWD) was developed. DLLME-HPLC-VWD is a method for determination of bisphenol A (BPA) in water samples. In this microextraction method, several parameters such as extraction solvent volume, sample volume, disperser solvent, ionic strength, pH, and disperser volume were optimised with the aid of interactive orthogonal array and a mixed level experiment design. First, an orthogonal array design was used to screen the significant variables for the optimisation. Second, the significant factors were optimised by using a mixed level experiment. Under the optimised extraction conditions (extraction solvent: ionic liquid [C6MIM][PF6], 60 µL; dispersive solvent: methanol, 0.4 mL; and pH = 4.0), the performance of the established method was evaluated. The response linearity of the method was observed in a range of 0.002–1.0 mg L−1 (three orders of magnitude) with correlation coefficient (R 2) of 0.9999. The repeatability of this method was 4.2–5.3% for three different BPA levels and the enrichment factors were above 180. The extraction recovery was about 50% for the three different concentrations with 3.4–6.4% of RSD. Limit of detection of the method was 0.40 µg L−1 at a signal-to-noise ratio of 3. In addition, the relative recovery of sample of Songhua River, tap water and barrel-drain water at different spiked concentration levels was ranged 95.8–103.0%, 92.6–98.6% and 87.2–95.3%, respectively. Compared with other extraction technologies, there have been the following advantages of quick, easy operation, and time-saving for the present method.

Preparation and characteristic of cobalt phthalocyanine modified carbon paste electrode for bisphenol A detection

Abstract In this paper, a simple and high sensitive electroananlytical method for determination of bisphenol A (BPA) by using cobalt phthalocyanine (CoPc) modified carbon paste electrode (CPE) was presented. The electrochemical oxidation behavior of BPA on the modified electrode was investigated by cyclic voltammetry (CV), chronocoulometry (CC), differential pulse voltammetry (DPV), linear sweep voltammetry (LSV), and bulk electrolysis with coulometry. Factors influencing the detection processes were optimized and kinetic parameters were calculated. Under the optimal conditions, the oxidation peak current was proportional to BPA concentration in the range of 8.75 × 10 −8 –1.25 × 10 −5 M with correlation coefficient 0.9987 and limits of detection 1.0 × 10 −8 M. The electrooxidation mechanisms of BPA on the electrode surface and the proposed method applied for detection of BPA in plastic products were also discussed.

Simple and Sensitive Electrochemiluminescence Method for Determination of Bisphenol a Based on its Inhibitory Effect on the Electrochemiluminescence of Luminol

AbstractAn electrochemiluminescence inhibition method has been developed for the determination of bisphenol A based on studying the inhibition phenomena of bisphenol A to the electrochemiluminescence of luminol. There is a linear relationship between the inhibitive intensity of electrochemiluminescence and the concentration of bisphenol A in the range of 4.4 × 10−7 to 2.2 × 10−5 mol/l. The method was successfully applied to the determination of bisphenol A in hot water in contact with commercially available table‐water bottle samples.