Skip to main content
SpringerLink
Log in

Simultaneous Determination of 16 Phthalate Esters in Suet Oil by GC–EIMS Coupled with Refrigerant Centrifugation and Ethylenediamine-N-propylsilane Depuration

  • Original
  • Published:
Chromatographia Aims and scope Submit manuscript

Abstract

Phthalic acid esters (PAEs) are endocrine-disrupting chemicals that can enter the human body easily via contaminated food and pharmaceutical excipients. The main challenge in the detection of PAEs in oily samples is not the choice of chromatography–mass spectrometry technology but the pretreatment method. Suet oil (SO), a fatty oil obtained from Capra hircus Linnaeus or Ovis aries Linnaeus, is widely used in food additives and the processing of Chinese medicine. In this paper, refrigerant centrifugation (RC) was optimized to pretreat SO samples for the separation of PAEs and fatty acids. Extraction with acetonitrile (n-hexane saturated) combined with RC (− 15 °C, 5000 rpm, 15 min, twice) was systematically assessed by four factors (temperature, time, speed, and frequency) according to response surface methodology. Gas chromatography–electron ionization quadrupole mass spectrometry (GC–EIMS) was used as an external standard method for quantification. The correlation coefficients of 16 PAEs were all 0.999 and the lowest quantified level was 0.1 mg kg−1. The recoveries of the 16 PAEs were 82.9–105.5% with relative standard deviations of 1.5–8.5% (n = 6). Compared with solid-phase extraction (SPE), RC had higher recovery rate, lower consumption (economy ratio 65.7%), and powerful sample processing ability. Results showed that the contents of di-n-butyl phthalate (DBP) in two batches of SO were higher than the official limit published by the Ministry of Public Health of China (0.3 mg kg−1). This study provides an alternative method for the determination of PAEs in SO and other edible or medicinal animal oil with wide practicability and less matrix interference.

This is a preview of subscription content, log in via an institution to check access.

Access this article

Log in via an institution

Price excludes VAT (USA)
Tax calculation will be finalised during checkout.

Instant access to the full article PDF.

Institutional subscriptions

Fig. 1
Fig. 2
Fig. 3
Fig. 4
Fig. 5

Similar content being viewed by others

References

  1. Shen Chen, Tong Wu, Zang Xiaohuan (2019) Hollow fiber stir bar sorptive extraction combined with GC–MS for the determination of phthalate esters from children’s food. Chromatographia 82:683–693

    Article  CAS  Google Scholar 

  2. Beltifa A, Feriani A, Machreki M, Ghorbel A, Ghazouani L, Di Bella G, Van Loco J, Reyns T, Mansour HB (2017) Plasticizers and bisphenol A, in packaged foods sold in the Tunisian markets: study of their acute in vivo toxicity and their environmental fate. Environ Sci Pollut Res Int 24(28):22382–22392

    Article  CAS  Google Scholar 

  3. Posnack NG, Idrees R, Ding H, Jaimes R 3rd, Stybayeva G, Karabekian Z, Laflamme MA, Sarvazyan N (2015) Exposure to phthalates affects calcium handling and intercellular connectivity of human stem cell-derived cardiomyocytes. PLoS One 10(3):e0121927

    Article  Google Scholar 

  4. Al-Saleh I, Elkhatib R, Al-Rajoudi T, Al-Qudaihi G (2017) Assessing the concentration of phthalate esters (PAEs) and bisphenol A (BPA) and the genotoxic potential of treated wastewater (final effluent) in Saudi Arabia. Sci Total Environ 578:440–451

    Article  CAS  Google Scholar 

  5. Li MC, Chen CH, Guo YL (2017) Phthalate esters and childhood asthma: a systematic review and congener-specific meta-analysis. Environ Pollut 229:655–660

    Article  CAS  Google Scholar 

  6. Ku HY, Su PH, Wen HJ, Sun HL, Wang CJ, Chen HY, Jaakkola JJ, Wang SL, TMICS Group (2015) Prenatal and postnatal exposure to phthalate esters and asthma: a 9-year follow-up study of a Taiwanese birth cohort. PLoS One 10(4):e0123309

    Article  Google Scholar 

  7. Jia LL, Lou XY, Guo Y, Leung KS, Zeng EY (2017) Occurrence of phthalate esters in over-the-counter medicines from China and its implications for human exposure. Environ Int 98:137–142

    Article  CAS  Google Scholar 

  8. Jiang J, Jia X (2015) Profiling of fatty acids composition in suet oil based on GC–EI–qMS and chemometrics analysis. Int J Mol Sci 16(2):2864–2878

    Article  CAS  Google Scholar 

  9. Chinese Pharmacopoeia Committee (2015) China Pharmacop 1:327–328

    Google Scholar 

  10. Cui L, Sun E, Zhang ZH, Tan XB, Wei YJ, Jin X, Jia XB (2012) Enhancement of epimedium fried with suet oil based on in vivo formation of self-assembled flavonoid compound nanomicelles. Molecules 17(11):12984–12996

    Article  CAS  Google Scholar 

  11. Jiang J, Li J, Zhang Z, Sun E, Feng L, Jia X (2015) Mechanism of enhanced antiosteoporosis effect of circinal-icaritin by self-assembled nanomicelles in vivo with suet oil and sodium deoxycholate. Int J Nanomed 10:2377–2389

    Article  CAS  Google Scholar 

  12. Jiang J, Feng L, Li J, Sun E, Ding SM, Jia XB (2014) Multielemental composition of suet oil based on quantification by ultrawave/ICP-MS coupled with chemometric analysis. Molecules 19(4):4452–4465

    Article  Google Scholar 

  13. Ebrahim K, Poursafa P, Amin MM (2017) Development of a simple and valid method for the trace determination of phthalate esters in human plasma using dispersive liquid–liquid microextraction coupled with gas chromatography–mass spectrometry. J Sep Sci 40(22):4403–4410

    Article  CAS  Google Scholar 

  14. Barp L, Purcaro G, Franchina FA, Zoccali M, Sciarrone D, Tranchida PQ, Mondello L (2015) Determination of phthalate esters in vegetable oils using direct immersion solid-phase microextraction and fast gas chromatography coupled with triple quadrupole mass spectrometry. Anal Chim Acta 887:237–244

    Article  CAS  Google Scholar 

  15. Fan JC, Jin Q, Zhang L, Huang XH, Ren R, Yang ZQ (2014) Simultaneous determination of 20 phthalate esters in oil-free food by UPLC/MS/MS. J AOAC Int 97(4):1151–1158

    Article  CAS  Google Scholar 

  16. Cinelli G, Avino P, Notardonato I, Centola A, Russo MV (2014) Study of XAD-2 adsorbent for the enrichment of trace levels of phthalate esters in hydroalcoholic food beverages and analysis by gas chromatography coupled with flame ionization and ion-trap mass spectrometry detectors. Food Chem 146:181–187

    Article  CAS  Google Scholar 

  17. Cinelli G, Avino P, Notardonato I, Centola A, Russo MV (2013) Rapid analysis of six phthalate esters in wine by ultrasound-vortex-assisted dispersive liquid–liquid micro-extraction coupled with gas chromatography-flame ionization detector or gas chromatography–ion trap mass spectrometry. Anal Chim Acta 769:72–78

    Article  CAS  Google Scholar 

  18. Russo MV, Notardonato I, Cinelli G, Avino P (2012) Evaluation of an analytical method for determining phthalate esters in wine samples by solid-phase extraction and gas chromatography coupled with ion-trap mass spectrometer detector. Anal Bioanal Chem 402(3):1373–1381

    Article  CAS  Google Scholar 

  19. Russo MV, Avino P, Notardonato I (2016) Fast analysis of phthalates in freeze-dried baby foods by ultrasound-vortex-assisted liquid–liquid microextraction coupled with gas chromatography–ion trap/mass spectrometry. J Chromatogr A 1474:1–7

    Article  CAS  Google Scholar 

  20. State Food and Drug Administration (2016) GB/T 21911-2008:2–7

  21. Liu Y, Wang S, Wang L (2013) Development of rapid determination of 18 phthalate esters in edible vegetable oils by gas chromatography tandem mass spectrometry. J Agric Food Chem 61(6):1160–1164

    Article  CAS  Google Scholar 

  22. Amanzadeh H, Yamini Y, Moradi M, Asl YA (2016) Determination of phthalate esters in drinking water and edible vegetable oil samples by headspace solid phase microextraction using graphene/polyvinylchloride nanocomposite coated fiber coupled to gas chromatography-flame ionization detector. J Chromatogr A 1465:38–46

    Article  CAS  Google Scholar 

  23. Barp L, Purcaro G, Franchina FA, Zoccali M, Sciarrone D, Tranchida PQ, Mondello L (2015) Determination of phthalate esters in vegetable oils using direct immersion solid-phase microextraction and fast gas chromatography coupled with triple quadrupole mass spectrometry. Anal Chim Acta 887:237–244

    Article  CAS  Google Scholar 

  24. Zeng F, Liu W, Jiang H, Yu HQ, Zeng RJ, Guo Q (2011) Separation of phthalate esters from bio-oil derived from rice husk by a basification–acidification process and column chromatography. Bioresour Technol 102(2):1982–1987

    Article  CAS  Google Scholar 

  25. Xie Q, Liu S, Fan Y, Sun J, Zhang X (2014) Determination of phthalate esters in edible oils by use of QuEChERS coupled with ionic-liquid-based dispersive liquid–liquid microextraction before high-performance liquid chromatography. Anal Bioanal Chem 406(18):4563–4569

    Article  CAS  Google Scholar 

  26. Sun H, Yang Y, Li H, Zhang J, Sun N (2012) Development of multiresidue analysis for twenty phthalate esters in edible vegetable oils by microwave-assisted extraction-gel permeation chromatography-solid phase extraction-gas chromatography–tandem mass spectrometry. J Agric Food Chem 60(22):5532–5539

    Article  CAS  Google Scholar 

  27. Lin Z, Zhang J, Cui H, Zhang L, Chen G (2010) Determination of phthalate esters in soil by microemulsion electrokinetic chromatography coupled with accelerated solvent extraction. J Sep Sci 33(23–24):3717–3725

    Article  CAS  Google Scholar 

  28. Guo Z, Wang S, Wei D, Wang M, Zhang H, Gai P, Duan J (2010) Development and application of a method for analysis of phthalates in ham sausages by solid-phase extraction and gas chromatography–mass spectrometry. Meat Sci 84(3):484–490

    Article  CAS  Google Scholar 

  29. Ros O, Vallejo A, Olivares M, Etxebarria N, Prieto A (2016) Determination of endocrine disrupting compounds in fish liver, brain, and muscle using focused ultrasound solid–liquid extraction and dispersive solid phase extraction as clean-up strategy. Anal Bioanal Chem 408(21):5689–5700

    Article  CAS  Google Scholar 

  30. Dargahi R, Ebrahimzadeh H, Asgharinezhad AA, Hashemzadeh A, Amini MM (2018) Dispersive magnetic solid-phase extraction of phthalate esters from water samples and human plasma based on a nanosorbent composed of MIL-101(Cr) metal-organic framework and magnetite nanoparticles before their determination by GC–MS. J Sep Sci 41(4):948–957

    Article  CAS  Google Scholar 

  31. Zhou X, Cui K, Zeng F, Li S, Zeng Z (2016) A simple and selective method for determination of phthalate biomarkers in vegetable samples by high pressure liquid chromatography–electrospray ionization–tandem mass spectrometry. Food Chem 200:336–342

    Article  CAS  Google Scholar 

  32. Wang H, Dong X, Jia B, Feng S, Liu J, Hongjian Z (2015) Determination of 23 phthalate esters in scallion and other vegetables by solid-phase extraction coupled with gas chromatography–tandem mass spectrometry. Se Pu 33(5):545–550

    CAS  PubMed  Google Scholar 

  33. Li S, Lin S, Chien YW, Daggy BP, Mirchandani HL (2001) Statistical optimization of gastric floating system for oral controlled delivery of calcium. AAPS PharmSciTech 2(1):E1

    Article  CAS  Google Scholar 

  34. Chang CW, Yen CC, Wu MT, Hsu MC, Wu YT (2017) Microwave-assisted extraction of cannabinoids in hemp nut using response surface methodology optimization and comparative study. Molecules 22(11):E1894

    Article  Google Scholar 

  35. Chen Y, Yin LZ, Zhao L, Shu G, Yuan ZX, Fu HL, Lv C, Lin JC (2017) Optimization of the ultrasound-assisted extraction of antioxidant phloridzin from Lithocarpus polystachyus Rehd. using response surface methodology. J Sep Sci 40(22):4329–4337

    Article  CAS  Google Scholar 

Download references

Acknowledgements

This work was supported by the National Natural Science Foundation of China (No. 81703773), Natural Science Foundation of Jiangsu Province (No. BK20170560 and BK20161075), China Postdoctoral Science Foundation (2018T110461).

Author information

Author notes

  1. Jun Jiang and Tong Chen contributed equally to this paper.

Authors and Affiliations

  1. School of Pharmacy, Jiangsu University, 301# Xuefu Road, Zhenjiang, 212013, Jiangsu, China

    Jun Jiang & Ximing Xu

  2. Comprehensive Technical Center, Zhenjiang Customs District P. R. of China, Zhenjing, 212004, China

    Tong Chen

Authors
  1. Jun Jiang
    View author publications

    You can also search for this author in PubMed Google Scholar

  2. Tong Chen
    View author publications

    You can also search for this author in PubMed Google Scholar

  3. Ximing Xu
    View author publications

    You can also search for this author in PubMed Google Scholar

Corresponding author

Correspondence to Ximing Xu.

Ethics declarations

Conflict of interest

All the authors declared that they had no conflict of interest.

Ethical Approval

This article does not contain any studies with human participants or animals performed by any of the authors.

Additional information

Publisher's Note

Springer Nature remains neutral with regard to jurisdictional claims in published maps and institutional affiliations.

Electronic supplementary material

Below is the link to the electronic supplementary material.

Supplementary material 1 (DOCX 4202 kb)

Rights and permissions

Reprints and permissions

About this article

Check for updates. Verify currency and authenticity via CrossMark

Cite this article

Jiang, J., Chen, T. & Xu, X. Simultaneous Determination of 16 Phthalate Esters in Suet Oil by GC–EIMS Coupled with Refrigerant Centrifugation and Ethylenediamine-N-propylsilane Depuration. Chromatographia 82, 1721–1732 (2019). https://doi.org/10.1007/s10337-019-03789-8

Download citation

  • Received:

  • Revised:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s10337-019-03789-8

Keywords

Search

Navigation