Abstract
Bisphenols (BPs) are hazardous organic chemicals showed endocrine disrupting activity, which has become a growing concern in the present era. In this study, a clean-up procedure, the QuEChERS method was optimized using the design of experiment (DOE) approach and combined with DLLME using acetone (disperser solvent) and 2-dodecanone (extraction solvent) for the quantitative determination of nine different BPs in plastic packed fruit juices. Prepared samples were analyzed by injector port silylation coupled with GC–MS/MS. Significant parameters were selected, viz., sodium acetate, PSA, and centrifugation time from the Pareto chart, and a further central composite design (CCD) experiment was performed to optimize the QuEChERS method. The calibration curve was obtained for concentration range of 0.78–100 ng mL−1, and a determination coefficient (R2) was found to be 0.9993. The range of LOD values was found in 0.31 to 1.71 ng mL−1. The procedure showed satisfactory precision (RSD ≤ 7.91%) and high extraction recoveries (92.69–112.06%). Finally, the developed method is applied for the quantitative analysis of BPs in packed fruit juices. The results show the presence of BPM, BPA, and BPS in the range of 1.10 to 47.08 ng/mL.
This is a preview of subscription content, log in via an institution to check access.
Similar content being viewed by others
Data Availability
The manuscript has obtained approval from the Institute, and a communication number was IITR/SEC/MS/2022/74. The raw data of analyzed samples during the study are available by the corresponding author on reasonable request.
References
Anastassiades M, Lehotay SJ, Stajnbaher D, Schenck FJ (2003) Fast and easy multiresidue method employing acetonitrile extraction/partitioning and “dispersive solid-phase extraction” for the determination of pesticide residues in produce. J AOAC Int 86:412–431. https://doi.org/10.1093/jaoac/86.2.412
Asati A, Satyanarayana G, Panchal S, Thakur RS, Ansari NG, Patel DK (2017) Ionic liquid based vortex assisted liquid–liquid microextraction combined with liquid chromatography mass spectrometry for the determination of bisphenols in thermal papers with the aid of response surface methodology. J Chromatogr A 1509:35–42. https://doi.org/10.1016/j.chroma.2017.06.040
Authority E (2015) Scientific opinion on the risks to public health related to the presence of bisphenol A (BPA) in foodstuffs. EFSA J, 13(1). https://doi.org/10.2903/j.efsa.2015.3978
Bazzano LA, Li TY, Joshipura KJ, Hu FB (2008) Intake of fruit, vegetables, and fruit juices and risk of diabetes in women. Diabetes Care 31:1311–1317. https://doi.org/10.2337/dc08-0080
Birnbaum LS, Bucher JR, Collman GW, Zeldin DC, Johnson AF, Schug TT, Heindel JJ (2012) Consortium-based science: the NIEHS’s multipronged, collaborative approach to assessing the health effects of bisphenol A. Environ Health Perspect 120:1640–1644. https://doi.org/10.1289/ehp.1205330
Cao P, Zhong HN, Qiu K, Li D, Wu G, Sui HX, Song Y (2021) Exposure to bisphenol A and its substitutes, bisphenol F and bisphenol S from canned foods and beverages on Chinese market. Food Control 120:107502. https://doi.org/10.1016/j.foodcont.2020.107502
Cunha S, Fernandes J (2013) Assessment of bisphenol A and bisphenol B in canned vegetables and fruits by gas chromatography–mass spectrometry after QuEChERS and dispersive liquid–liquid microextraction. Food Control 33:549–555. https://doi.org/10.1016/j.foodcont.2013.03.028
Deming SN, Morgan SL (1993) Experimental design: a chemometric approach. Elsevier
Ehrlich S, Williams PL, Missmer SA, Flaws JA, Berry KF, Calafat AM, Ye X, Petrozza JC, WrightD HR (2012) Urinary bisphenol A concentrations and implantation failure among women undergoing in vitro fertilization. Environ Health Perspect 120:978–983. https://doi.org/10.1289/ehp.1104307
Eladak S, Grisin T, Moison D, Guerquin MJ, N’Tumba-Byn T, Pozzi-Gaudin S, Benachi A, Livera G, Rouiller-Fabre V, Habert R (2015) A new chapter in the bisphenol A story: bisphenol S and bisphenol F are not safe alternatives to this compound. Fertil Steril 103:11–21. https://doi.org/10.1016/j.fertnstert.2014.11.005
Gallo P, Di Marco PI, Fattore M, Rimoli MG, Seccia S, Albrizio S (2019) A method to determine BPA, BPB, and BPF levels in fruit juices by liquid chromatography coupled to tandem mass spectrometry. Food Addit Contam 36:1871–1881. https://doi.org/10.1080/19440049.2019.1657967
Gao G, Chen H, Zhu L, Chai Y, Ma G, Wang C, Hao Z, Liu X, Lu C (2017) Simultaneous determination of bisphenol A and tetrabromobisphenol A in tea using a modified QuEChERS sample preparation method coupled with liquid chromatography-tandem mass spectrometry. Anal Methods 9:6769–6776. https://doi.org/10.1039/C7AY02145C
Guideline IHT (2022) validation of analytical procedures Q2 (R1). International Conference of Harmonization: Switzerland Geneva
Khan MR, Ouladsmane M, Alammari AM, Azam M (2021) Bisphenol A leaches from packaging to fruit juice commercially available in markets. Food Packag 28:100678. https://doi.org/10.1016/j.fpsl.2021.100678
Li Y, Burns KA, Arao Y, Luh CJ, Korach KS (2012) Differential estrogenic actions of endocrine-disrupting chemicals bisphenol A bisphenol AF, and zearalenone through estrogen receptor α and β in vitro. Envrion Health Perspect 120:1029–1035. https://doi.org/10.1289/ehp.1104689
Li J, Zhou H, Liu YX, Yan XY, Xu YP, Liu SM (2014) Solid-phase extraction for selective determination of bisphenol A in drinks and fruits by dummy surface molecularly imprinted polymer with direct synthetic method. Food Addit Contam Part A 31:1139–1146. https://doi.org/10.1080/19440049.2014.906751
Liao C, Kannan K (2013) Concentrations and profiles of bisphenol A and other bisphenol analogues in foodstuffs from the United States and their implications for human exposure. J Agric Food Chem 61:4655–4662. https://doi.org/10.1021/jf400445n
Lippi G, Blanckaert N, Bonini P, Green S, Kitchen S, Palicka V, Vassault AJ, Plebani M (2008) Haemolysis: an overview of the leading cause of unsuitable specimens in clinical laboratories. Clin Chem Lab Med 46:764–772. https://doi.org/10.1515/CCLM.2008.170
Loh SH, Ong ST, Ngu ML, Mohd Ariffin M (2017) Rapid extraction of bisphenol A by dispersive liquid-liquid microextraction based on solidification of floating organic. Sains Malaysiana 46:615–621. https://doi.org/10.17576/jsm-2017-4604-14
Mandrah K, Satyanarayana G, Roy SK (2017) A dispersive liquid-liquid microextraction based on solidification of floating organic droplet followed by injector port silylation coupled with gas chromatography–tandem mass spectrometry for the determination of nine bisphenols in bottled carbonated beverages. J Chromatogr A 1528:10–17. https://doi.org/10.1016/j.chroma.2017.10.071
Meeker JD, Ehrlich S, Toth TL, Wright DL, Calafat AM, Trisini AT, Xiaoyum Ye, Hauser R (2010) Semen quality and sperm DNA damage in relation to urinary bisphenol A among men from an infertility clinic. Reprod Toxicol 30:532–539. https://doi.org/10.1016/j.reprotox.2010.07.005
Oyejola B, Nwanya J (2015) Selecting the right central composite design. Int J Stat Manag Syst 5:21–30. https://doi.org/10.5923/j.statistics.20150501.04
Plössl F, Giera M, Bracher F (2006) Multiresidue analytical method using dispersive solid-phase extraction and gas chromatography/ion trap mass spectrometry to determine pharmaceuticals in whole blood. J Chromatogr A 1135:19–26. https://doi.org/10.1016/j.chroma.2006.09.033
Regueiro J, Wenzl T (2015) Determination of bisphenols in beverages by mixed-mode solid-phase extraction and liquid chromatography coupled to tandem mass spectrometry. J Chromatogr A 1422:230–238. https://doi.org/10.1016/j.chroma.2015.10.046
Rizzetti TM, Kemmerich M, Martins ML, Prestes OD, Adaime MB, Zanella R (2016) Optimization of a QuEChERS based method by means of central composite design for pesticide multiresidue determination in orange juice by UHPLC–MS/MS. Food Chem 196:25–33. https://doi.org/10.1016/j.foodchem.2015.09.010
Vandenberg LN, Maffini MV, Sonnenschein C, Rubin BS, Soto AM (2009) Bisphenol-A and the great divide: a review of controversies in the field of endocrine disruption. Endor. Rev. 30:75–95. https://doi.org/10.1210/er.2008-0021
Vom Saal FS, Myers JP (2008) Bisphenol A and risk of metabolic disorders. JAMA 300:1353–1355. https://doi.org/10.1001/jama.300.11.1353
Wang Q, Ma L, Yin CR, Xu L (2013) Developments in injection port derivatization. J Chromatogr A 1296:25–35. https://doi.org/10.1016/j.chroma.2013.04.036
Wang XC, Shu B, Li S, Yang ZG, Qiu B (2017) QuEChERS followed by dispersive liquid–liquid microextraction based on solidification of floating organic droplet method for organochlorine pesticides analysis in fish. Talanta 162:90–97. https://doi.org/10.1016/j.talanta.2016.09.069
Welshons WV, Nagel SC, vom Saal FS (2006) Large effects from small exposures. III. Endocrine mechanisms mediating effects of bisphenol A at levels of human exposure. Endocrinology 147:56-s69. https://doi.org/10.1210/en.2005-1159
Wolff MS (2006) Endocrine disruptors: challenges for environmental research in the 21st century. Ann. N.Y. Acad Sci 1076:228–238. https://doi.org/10.1196/annals.1371.009
Yang Y, Yu J, Yin J, Shao B, Zhang J (2014) Molecularly imprinted solid-phase extraction for selective extraction of bisphenol analogues in beverages and canned food. J Agric Food Chem 62:11130–11137. https://doi.org/10.1021/jf5037933
Zhou Q, Gao Y, Xie G (2011) Determination of bisphenol A, 4-n-nonylphenol, and 4-tert-octylphenol by temperature-controlled ionic liquid dispersive liquid-phase microextraction combined with high performance liquid chromatography-fluorescence detector. Talanta 85:1598–1602. https://doi.org/10.1016/j.talanta.2011.06.050
Zhou J, Chen XH, Pan SD, Wang JL, Zheng YB, Xu JJ, Zhao YG, Cai ZX, Jin MC (2019) Contamination status of bisphenol A and its analogues (bisphenol S, F and B) in foodstuffs and the implications for dietary exposure on adult residents in Zhejiang Province. Food Chem 294:160–170. https://doi.org/10.1016/j.foodchem.2019.05.022
Funding
UP-CST (CST/1588) funded the current study.
Author information
Authors and Affiliations
Contributions
V.J. performed experiments for this study. V.J. developed techniques including extraction and sample preparation for the BPs analogs analysis in the fruit juice sample. V.J. and I.G. wrote the manuscript. R.V. and I.G. helped in sample preparation and performed experiments for this study. S.K.R. Designed, supervised, executed, and coordinated this whole study. S.K.R. wrote and corrected the manuscript.
Corresponding author
Ethics declarations
Competing Interests
The authors declare no competing interests.
Conflict of Interest
Veena Jain declares that she has no conflict of interest. Rahul Verma declares that he has no conflict of interest. Iti Gaur declares that he has no conflict of interest. Somendu Kumar Roy declares that he has no conflict of interest.
Additional information
Publisher's Note
Springer Nature remains neutral with regard to jurisdictional claims in published maps and institutional affiliations.
Supplementary Information
Below is the link to the electronic supplementary material.
Rights and permissions
Springer Nature or its licensor (e.g. a society or other partner) holds exclusive rights to this article under a publishing agreement with the author(s) or other rightsholder(s); author self-archiving of the accepted manuscript version of this article is solely governed by the terms of such publishing agreement and applicable law.
About this article
Cite this article
Jain, V., Verma, R., Gaur, I. et al. Design of Experiment Approach to Assess Nine Bisphenols in Fruit Juice Using QuEChERS with Injector Port Silylation via GC–MS/MS. Food Anal. Methods 16, 1370–1380 (2023). https://doi.org/10.1007/s12161-023-02503-7
Received:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1007/s12161-023-02503-7