Comparison of DAD and FLD Detection for Identification of Selected Bisphenols in Human Breast Milk Samples and Their Quantitative Analysis by LC-MS/MS.
J AOAC Int. 2020 Jul 01; 103(4):1029-1042.JA

Abstract

BACKGROUND

Determination of bisphenols released from packaging material is undoubtedly a difficult and tricky task, requiring the chemical analyst to develop an individual approach to obtain reliable analytical information.

OBJECTIVE

QuECHERS (Quick, Easy, Cheap, Effective, Rugged, and Safe)/dispersive solid-phase extraction (d-SPE) technique and high performance liquid chromatography (HPLC) coupled with modern detection techniques such as diode-array detector (DAD), ﬂuorescence detector (FLD) or tandem mass spectrometry (MS/MS) for the determination of bisphenols such as bisphenol A (BPA), bisphenol S (BPS), bisphenol F (BPF), bisphenol B (BPB), 2-[[4-[2-[4-(Oxiran-2-ylmethoxy)phenyl]propan-2yl]phenoxy] methyl]oxirane (BADGE), 3-[4-[2-[4-(Oxiran-2-ylmethoxy)phenyl]propan-2-yl]phenoxy]propane-1,2-diol (BADGE*H2O), 3-[4-[2-[4-(2,3-Dihydroxypropoxy)phenyl]propan-2-yl]phenoxy]propane-1,2-diol (BADGE*2H2O), 1-Chloro-3-[4-[2-[4-(3-chloro-2-hydroxypropoxy)phenyl] propan-2-yl]phenoxy]propan-2-ol (BADGE*2HCl) in human breast milk samples have been performed.

METHODS

For the analysis of total analytes, prior to the extraction with acetonitrile, a deconjugation step was implemented in a tube by adding 1 mL of the enzymatic solution with the β-Glucuronidase to 5 mL of sample. The mix was homogenized and incubated for 17 h at 37°C. Ten milliliters of acetonitrile, and a QuEChERS salt packet with 4 g anhydrous MgSO4 and 1 g NaCl were added. During the d-SPE step the extract was transferred into tube with 30 mg Z-Sep and 50 mg PSA (and also 150 mg MgSO4 for LC-MS/MS analysis). MeOH-water (20:80, v/v) were added to the dry residue and the extract was reconstituted in 150 µL (25-fold analytes pre-concentration is achieved). Next bisphenols were identified by HPLC-DAD-FLD and quantified by LC-MS/MS equipment.

CONCLUSIONS

During the bisphenols HPLC-DAD-FLD analysis, from 6 min a reinforcement of 15 was used, which allowed analytes to be identified at 750 pg/mL. Application of LC-MS/MS allowed quantification of bisphenols in the range from 2.12 to 116.22 ng/mL in a total 27 human breast milk samples.

HIGHLIGHTS

First QuEChERS/d-SPE coupled with HPLC-DAD-FLD or LC-MS/MS method for the quantification of bisphenols and its analogues in breast milk Faster and cheaper alternative to traditional extraction methods The method was applied for the first biomonitoring of bisphenols and its analogues in breast milk.

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Authors+Show Affiliations

Tuzimski T

Medical University of Lublin, Department of Physical Chemistry, 4A Chodzki Street, 20-093 Lublin, Poland.

Szubartowski S

Medical University of Lublin, Department of Physical Chemistry, 4A Chodzki Street, 20-093 Lublin, Poland.

Gadzała-Kopciuch R

Nicolaus Copernicus University in Toruń, Faculty of Chemistry, Department of Environmental Chemistry and Bioanalytics, 7 Gagarin St, 87 100 Toruń, Poland. Interdisciplinary Centre of Modern Technologies, Nicolaus Copernicus University in Toruń, 4 Wileńska St, 87-100 Toruń, Poland.

Miturski A

Medical University of Lublin, Department of Obstetrics and Pathology of Pregnancy, 16 Staszica Street, 20-081 Lublin, Poland.

Wójtowicz-Marzec M

Medical University of Lublin, Department of Obstetrics and Pathology of Pregnancy, 16 Staszica Street, 20-081 Lublin, Poland.

Kwaśniewski W

Medical University of Lublin, Department of Gynaecological Oncology and Gynaecology, 16 Staszica Street, 20-081 Lublin, Poland.

Buszewski B

MeSH

Benzhydryl CompoundsChromatography, LiquidFemaleHumansMilk, HumanPhenolsSolid Phase ExtractionTandem Mass Spectrometry

Pub Type(s)

Journal Article

Language

eng

PubMed ID

33241324

Citation

Tuzimski, Tomasz, et al. "Comparison of DAD and FLD Detection for Identification of Selected Bisphenols in Human Breast Milk Samples and Their Quantitative Analysis By LC-MS/MS." Journal of AOAC International, vol. 103, no. 4, 2020, pp. 1029-1042.

Tuzimski T, Szubartowski S, Gadzała-Kopciuch R, et al. Comparison of DAD and FLD Detection for Identification of Selected Bisphenols in Human Breast Milk Samples and Their Quantitative Analysis by LC-MS/MS. J AOAC Int. 2020;103(4):1029-1042.

Tuzimski, T., Szubartowski, S., Gadzała-Kopciuch, R., Miturski, A., Wójtowicz-Marzec, M., Kwaśniewski, W., & Buszewski, B. (2020). Comparison of DAD and FLD Detection for Identification of Selected Bisphenols in Human Breast Milk Samples and Their Quantitative Analysis by LC-MS/MS. Journal of AOAC International, 103(4), 1029-1042. https://doi.org/10.1093/jaoacint/qsaa027

Tuzimski T, et al. Comparison of DAD and FLD Detection for Identification of Selected Bisphenols in Human Breast Milk Samples and Their Quantitative Analysis By LC-MS/MS. J AOAC Int. 2020 Jul 1;103(4):1029-1042. PubMed PMID: 33241324.

* Article titles in AMA citation format should be in sentence-case

TY - JOUR T1 - Comparison of DAD and FLD Detection for Identification of Selected Bisphenols in Human Breast Milk Samples and Their Quantitative Analysis by LC-MS/MS. AU - Tuzimski,Tomasz, AU - Szubartowski,Szymon, AU - Gadzała-Kopciuch,Renata, AU - Miturski,Andrzej, AU - Wójtowicz-Marzec,Monika, AU - Kwaśniewski,Wojciech, AU - Buszewski,Bogusław, PY - 2019/10/09/received PY - 2020/02/17/revised PY - 2020/02/17/accepted PY - 2020/11/26/entrez PY - 2020/11/27/pubmed PY - 2021/6/29/medline SP - 1029 EP - 1042 JF - Journal of AOAC International JO - J AOAC Int VL - 103 IS - 4 N2 - BACKGROUND: Determination of bisphenols released from packaging material is undoubtedly a difficult and tricky task, requiring the chemical analyst to develop an individual approach to obtain reliable analytical information. OBJECTIVE: QuECHERS (Quick, Easy, Cheap, Effective, Rugged, and Safe)/dispersive solid-phase extraction (d-SPE) technique and high performance liquid chromatography (HPLC) coupled with modern detection techniques such as diode-array detector (DAD), ﬂuorescence detector (FLD) or tandem mass spectrometry (MS/MS) for the determination of bisphenols such as bisphenol A (BPA), bisphenol S (BPS), bisphenol F (BPF), bisphenol B (BPB), 2-[[4-[2-[4-(Oxiran-2-ylmethoxy)phenyl]propan-2yl]phenoxy] methyl]oxirane (BADGE), 3-[4-[2-[4-(Oxiran-2-ylmethoxy)phenyl]propan-2-yl]phenoxy]propane-1,2-diol (BADGE*H2O), 3-[4-[2-[4-(2,3-Dihydroxypropoxy)phenyl]propan-2-yl]phenoxy]propane-1,2-diol (BADGE*2H2O), 1-Chloro-3-[4-[2-[4-(3-chloro-2-hydroxypropoxy)phenyl] propan-2-yl]phenoxy]propan-2-ol (BADGE*2HCl) in human breast milk samples have been performed. METHODS: For the analysis of total analytes, prior to the extraction with acetonitrile, a deconjugation step was implemented in a tube by adding 1 mL of the enzymatic solution with the β-Glucuronidase to 5 mL of sample. The mix was homogenized and incubated for 17 h at 37°C. Ten milliliters of acetonitrile, and a QuEChERS salt packet with 4 g anhydrous MgSO4 and 1 g NaCl were added. During the d-SPE step the extract was transferred into tube with 30 mg Z-Sep and 50 mg PSA (and also 150 mg MgSO4 for LC-MS/MS analysis). MeOH-water (20:80, v/v) were added to the dry residue and the extract was reconstituted in 150 µL (25-fold analytes pre-concentration is achieved). Next bisphenols were identified by HPLC-DAD-FLD and quantified by LC-MS/MS equipment. CONCLUSIONS: During the bisphenols HPLC-DAD-FLD analysis, from 6 min a reinforcement of 15 was used, which allowed analytes to be identified at 750 pg/mL. Application of LC-MS/MS allowed quantification of bisphenols in the range from 2.12 to 116.22 ng/mL in a total 27 human breast milk samples. HIGHLIGHTS: First QuEChERS/d-SPE coupled with HPLC-DAD-FLD or LC-MS/MS method for the quantification of bisphenols and its analogues in breast milk Faster and cheaper alternative to traditional extraction methods The method was applied for the first biomonitoring of bisphenols and its analogues in breast milk. SN - 1944-7922 UR - https://www.unboundmedicine.com/medline/citation/33241324/Comparison_of_DAD_and_FLD_Detection_for_Identification_of_Selected_Bisphenols_in_Human_Breast_Milk_Samples_and_Their_Quantitative_Analysis_by_LC_MS/MS_ DB - PRIME DP - Unbound Medicine ER -

Tags

Comparison of DAD and FLD Detection for Identification of Selected Bisphenols in Human Breast Milk Samples and Their Quantitative Analysis by LC-MS/MS.J AOAC Int. 2020 Jul 01; 103(4):1029-1042.JA