scholarly journals A Method Validation for Simultaneous Determination of Phthalates and Bisphenol A Released from Plastic Water Containers

2019 ◽  
Vol 9 (14) ◽  
pp. 2945 ◽  
Author(s):  
Ivan Notardonato ◽  
Carmela Protano ◽  
Matteo Vitali ◽  
Badal Bhattacharya ◽  
Pasquale Avino

Phthalates (or phthalate esters, PAEs) and bisphenol A (BPA) are widely used in various industries, particularly in the fields of cosmetics and packaging, and they increase the malleability and workability of materials. As a result of their use, some international health organizations have begun to study them. In this study, the authors developed a methodology for the simultaneous determination of dimethyl phthalate (DMP), diethyl phthalate (DEP), diisobutyl phthalate (DiBP); dibutyl phthalate (DBP), bis(2-ethylhexyl) phthalate (DEHP); di-n-octyl-phthalate (DnOP) and bisphenol A (BPA) from drinking and non-potable waters. The extraction of PAEs and BPA was performed using a solvent-based dispersive liquid–liquid microextraction (SB-DLLME) method. The analytical determination was performed using a gas chromatography–ion trap mass spectrometry (GC-IT/MS) analysis. The entire procedure was validated as recoveries were studied according to the volume and the extraction solvent used, pH, and ionic strength. Dynamic linearity ranges and linear equations of all the compounds were experimentally determined as well as the limit of detection (LOD) (1–8 ng mL−1) and the limit of quantification (LOQ) (5–14 ng mL−1), reproducibility, and sensitivity. The method was applied to 15 water samples (mineral water and tap water) for determining PAEs and BPA released from the plastic container. After the release simulation, four PAEs (i.e., DiBP, DBP, DHEP, and DnOP) were determined at very low concentrations (below 1.2 ng mL−1) in two water samples from (sport) bottles.

2020 ◽  
Vol 3 (1) ◽  
pp. 23 ◽  
Author(s):  
Ivan Notardonato ◽  
Sergio Passarella ◽  
Giuseppe Ianiri ◽  
Cristina Di Fiore ◽  
Mario Vincenzo Russo ◽  
...  

In this paper, an analytical protocol was developed for the simultaneous determination of phthalates (di-methyl phthalate DMP, di-ethyl phthalate DEP, di-isobutyl phthalate DiBP, di-n-butyl phthalate DBP, bis-(2-ethylhexyl) phthalate DEHP, di-n-octyl phthalate DNOP) and bisphenol A (BPA). The extraction technique used was the ultrasound vortex assisted dispersive liquid–liquid microextraction (UVA-DLLME). The method involves analyte extraction using 75 µL of benzene and subsequent analysis by gas chromatography combined with ion trap mass spectrometry (GC-IT/MS). The method is sensitive, reliable, and reproducible with a limit of detection (LOD) below 13 ng g−1 and limit of quantification (LOQ) below 22 ng g−1 and the intra- and inter-day errors below 7.2 and 9.3, respectively. The method developed and validated was applied to six honey samples (i.e., four single-use commercial ones and two home-made ones. Some phthalates were found in the samples at concentrations below the specific migration limits (SMLs). Furthermore, the commercial samples were subjected to two different thermal stresses (24 h and 48 h at 40 °C) for evidence of the release of plastic from the containers. An increase in the phthalate concentrations was observed, especially during the first phase of the shock, but the levels were still within the limits of the regulations.


2019 ◽  
pp. 332-337
Author(s):  
Gorica Vukovic ◽  
Marina Djukic ◽  
Tijana Stojanovic ◽  
Vojislava Bursic ◽  
Aleksandra Petrovic ◽  
...  

Bisphenol A is a monomer used primarily in the production of polycarbonate plastics and epoxy resins. Polycarbonate plastic is used in a wide variety of digital media products, electrical and electronic equipment, sport safety equipment, reusable food and drink containers, etc. Epoxy resins are used in engineering applications, paints and adhesives and also in a variety of protective coatings in metal cans for foods, bottle tops and water supply pipes. The content of BPA was evaluated in 16 samples (6 baby bottles and 10 drinking containers - can) collected during 2018/2019, of which three baby bottles and 8 cans were collected in 2018, while three baby bottles and 2 cans in 2019. A simple HPLC-FLD analytical method was validated for the quantitation of BPA from baby feeding bottles and cans. The separation was performed on a C18 column. Good linearity was obtained over the concentration range of 0.3-6.0 ?g/mL with the regression coefficient (R2) of 0.9998. The limit of detection (LOD) and limit of quantification (LOQ) were 0.01 and 0.03 ?g/mL, respectively. The repeatability of the method (%RSD) was between 4 and 6%, while the recovery ranged from 104.3 to 109.7%. The extraction of BPA was done in accordance with SRPS EN 13130-1:2008. The methods were applied to determine BPA release from baby bottles, performing repeated procedures according to EU and national regulations (SRPS CEN/TS 13130-13 (2008)). The conformity was evaluated according to National and EU requirements. The results show that Bisphenol-A was not detectable in any of the analysed samples.


2011 ◽  
Vol 11 (1) ◽  
pp. 55-60 ◽  
Author(s):  
J. Zheng ◽  
S. Q. Zhao ◽  
X. T. Xu ◽  
K. Zhang

In order to study whether bisphenol A (BPA) can pass into drinking water from polycarbonate barrel and exist in the river and industrial effluent the indirect competitive enzyme-linked immunosorbent assay (ELISA) for the determination of BPA was established. The results presented an inhibition concentration at 50% absorbance (IC50) of 0.123 mg L−1, and the limit of detection (LOD) is 9.934 μg L−1. The specificity of antiserum was proved well because the cross-reactivity with benzene, tert-butylbenzene, hydroquinone and o-hydroxybenzoic acid were found lower than 0.01%, except phenol was 0.26%. The method was found to be reliable and repeatable. It was used for monitoring the concentration of BPA in the barreled drinking water. The results confirmed BPA can pass into barreled drinking water from the polycarbonate barrel and concentration increased as days went on. A certain content of BPA was found in industrial effluent. The results of ELISA were consistent with the results of UV spectrophotometry. BPA could not be found in the water samples obtained from Zhujiang River. The established method shows specific recognition of BPA and could be applied in detection of environmental BPA.


2012 ◽  
Vol 31 (1) ◽  
pp. 39 ◽  
Author(s):  
Lenče Velkoska-Markovska ◽  
Biljana Petanovska-Ilievska ◽  
Lila Vodeb

A fast, simple, precise and accurate reversed-phase high-performance liquid chromatography (RPHPLC)method with UV-DAD for simultaneous determination of desmedipham, phenmedipham and ethofumesate in the pesticide formulation “Inter OF” has been developed. The analysis was performed on a LiChrospher 60 RP-select B (25 cm × 0.4 cm, 5 μm, Merck) analytical column, with mobile phase of methanol/water (60/40, V/V), flow rate of 1 ml/min, UV-detection at 230 nm and constant column temperature at 25 ºC. The following parameters were determined for the developed method: retention factor, separation factor, limit of detection (LOD), limit of quantification (LOQ), precision of obtained results for peak area, linearity, recovery of analyte and active ingredients quantity in a pesticide formulation.


2015 ◽  
Vol 7 (23) ◽  
pp. 9825-9834 ◽  
Author(s):  
Slobodan V. Jovanovic ◽  
Thomas Zakharov ◽  
Hemendra Mulye ◽  
Duck Kim ◽  
Kelly-Anne Fagan

In this study, we developed and validated a sensitive method for the determination of hydrazine in water samples using ion chromatography coupled with an amperometric detector (limit of detection (LOD) = 0.02 μg L−1 and limit of quantification (LOQ) = 0.1 μg L−1).


2016 ◽  
Vol 10 (1) ◽  
pp. 33-43 ◽  
Author(s):  
Najmul Hasan ◽  
Mathurot Chaiharn ◽  
Umair Ali Toor ◽  
Zulfiqar Ali Mirani ◽  
Ghulam Sajjad ◽  
...  

In this article we describe development and validation of stability indicating, accurate, specific, precise and simple Ion-pairing RP-HPLC method for simultaneous determination of paracetamol and cetirizine HCl along with preservatives i.e. propylparaben, and methylparaben in pharmaceutical dosage forms of oral solution and in serum. Acetonitrile: Buffer: Sulfuric Acid (45:55:0.3 v/v/v) was the mobile phase at flow rate 1.0 mL min-1 using a Hibar® Lichrosorb® C18 column and monitored at wavelength of 230nm. The averages of absolute and relative recoveries were found to be 99.3%, 99.5%, 99.8% and 98.7% with correlation coefficient of 0.9977, 0.9998, 0.9984, and 0.9997 for cetirizine HCl, paracetamol, methylparaben and Propylparaben respectively. The limit of quantification and limit of detection were in range of 0.3 to 2.7 ng mL-1 and 0.1 to 0.8 ng mL-1 respectively. Under stress conditions of acidic, basic, oxidative, and thermal degradation, maximum degradation was observed in basic and oxidative stress where a significant impact was observed while all drugs were found almost stable in the other conditions. The developed method was validated in accordance with ICH and AOAC guidelines. The proposed method was successfully applied to quantify amount of paracetamol, cetirizine HCl and two most common microbial preservatives in bulk, dosage form and physiological fluid.


2008 ◽  
Vol 5 (4) ◽  
pp. 706-712 ◽  
Author(s):  
A. V. Sulebhavikar ◽  
U. D. Pawar ◽  
K. V. Mangoankar ◽  
N. D. Prabhu-Navelkar

A rapid and simple high performance thin layer chromatography (HPTLC) method with densitometry at λ=263 nm was developed and validated for simultaneous determination of lopinavir and ritonavir from pharmaceutical preparation. Separation was performed on aluminum-backed silica gel 60F254HPTLC plates as stationary phase and using a mobile phase comprising of toluene, ethyl acetate, methanol and glacial acetic acid, in the volume ratio of 7.0:2.0:0.5:0.5 (v/v) respectively. After development, plates were observed under UV light. The detector response was linear in the range of 6.67 to 20.00 µg/spot and 1.67 to 5.00 µg/spot for lopinavir and ritonavir respectively. The validated lowest limit of detection was 21.00 ng/spot and 5.10 ng/spot whereas lowest limit of quantification was 7.00 ng/spot and 21.00 ng/spot for lopinavir and ritonavir respectively. The percentage assay of lopinavir and ritonavir was found between 98.23 to 102.28% and 98.03 to 103.50% respectively. The described method has the advantage of being rapid and easy. Hence it can be applied for routine quality control analysis of lopinavir and ritonavir from pharmaceutical preparation and stability studies.


2019 ◽  
Vol 2019 ◽  
pp. 1-6
Author(s):  
Ruth Rodriguez ◽  
Elianna Castillo ◽  
Diana Sinuco

A simple and economic high-performance liquid chromatography (HPLC-UV-Vis) analytical method was validated for the quantitation of specific Bisphenol-A migration from baby feeding bottles. Overall and specific migration assays were done with different food simulating matrices using the filling method. Good linearity was obtained over the concentration range of 0.01–0.6 mg/kg. The limit of detection (LOD) and limit of quantification (LOQ) were 0.004 and 0.010 mg/kg, respectively. The repeatability of the method (%RSD, n=10) was between 89.5 and 99.0%, while recovery ranged from 83.2 to 98.4%. The method was applied to specific migration assays from baby feeding bottles purchased from different plastic producers in Colombia. The results show that, in a first migration assay, Bisphenol-A was not detectable in all samples. In a second migration test, Bisphenol-A concentrations were higher than the most restricted limit (0.05 mg/kg) with ethanol 95% and isooctane as food simulants.


2015 ◽  
Vol 7 (5) ◽  
pp. 2121-2128 ◽  
Author(s):  
Parisa Sharifian ◽  
Alireza Aliakbar

Method and conditions: determination of trace amounts of Se(IV) by adsorptive cathodic stripping voltammetry at the Bi/Hg film electrode in an open circuit system; limit of detection: 0.07 ng mL−1; limit of quantification: 0.25 ng mL−1; RSD: 2.4% (for five replications of 5 ng mL−1 of Se(iv)); analytical range: 2–50 ng mL−1; interference: selective for Se(iv) – no interference; application: determination of Se(iv) in vegetable, fruits and water samples.


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