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Determination of low-level ink photoinitiator residues in packaged milk by solid-phase extraction and LC-ESI/MS/MS using triple-quadrupole mass analyzer

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Abstract

A confirmatory and quantitative method based on liquid chromatography–electrospray ionization tandem mass spectrometry (LC-ESI/MS/MS) has been developed for simultaneous determination of seven photoinitiator residues: benzophenone, (1-hydroxycyclohexyl)phenylketone (Irgacure 184), isopropylthioxanthone (ITX), 2-ethylhexyl-(4-dimethylamino)benzoate (EHA or EHDAB), 2-methyl-1-[4-(methylthio)phenyl]-2-(4-morpholinyl)-1-propanone (Irgacure 907), (2,4,6-trimethylbenzoyl)diphenylphosphine oxide (TPO) and 2-benzyl-2-(dimethylamino)-1-(4-morpholinophenyl)-1-butanone (Irgacure 369) in packaged milk and related packaging materials. Residues of photoinitiators were extracted from milk using acetonitrile, and further enriched and purified on HLB solid-phase extraction cartridges prior to being analyzed by LC-ESI/MS/MS with selected reaction monitoring mode, while photoinitiators in packaging materials were extracted using the same solvent. Satisfactory recovery (from 80 to 111%), intra- and inter-day precision (below 12%), and low limits of quantification (from 0.1 to 5.0 μg kg−1) were evaluated from spiked samples at three concentration levels (5.0, 10.0 and 25.0 μg kg−1 for Irgacure 184 and 2.5, 5.0 and 25.0 μg kg−1 for others). These excellent validation data suggested the possibility of using the LC-ESI/MS/MS method for simultaneous determination of low-level photoinitiator residues migrating from printed food-packaging materials into milk. The method has been successfully applied to the analysis of real samples of different fat contents ranging from 8 to 30 g L−1. The photoinitiator residues were revealed to be higher in milk with higher fat content and the most important contaminations were benzophenone and ITX in concentration ranges of 2.84–18.35 and 0.83–8.87 μg kg−1, respectively.

Recoveries of photoinitiators dealt with different kinds of elution solvents in solid-phase extraction process

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References

  1. Nestle and the ITX Recall (2005) Nestle Company. http://www.nestle.com/Media_Center/ITXrecall23Nov05.htm. 2005-11-24

  2. Opinion of the Scientific Panel of Food Additives, Flavourings, Processing Aids and Materials in contact with food on a request from the commission related to 2-isopropyl thioxanthone (ITX) and 2-ethylhexyl-4-dimethylaminobenzoate (EHDAB) in food contact materials (2005) EFSA

  3. Sagratini G, Manes J, Giardina D, Pico Y (2006) J Agric Food Chem 54:7947–7952

    Article  CAS  Google Scholar 

  4. Commission Decision 2002/657/EC of 12 August 2002 implementing Council Directive 96/23/EC concerning the performance of analytical methods and the interpretation of results. Off J Eur Communities 2002, L221:8-36

    Google Scholar 

  5. Sagratini G, Caprioli G, Cristalli G, Giardina D, Ricciutelli M, Volpini R, Zuo YT, Vittori S (2008) J Chromatogr A 1194:213–220

    Article  CAS  Google Scholar 

  6. Morlock G, Schwack W (2006) Anal Bioanal Chem 385:586–595

    Article  CAS  Google Scholar 

  7. Bagnati R, Bianchi G, Marangon E, Zuccato E, Fanelli R, Davoli E (2007) Rapid Commun Mass Spectrom 21:1998–2002

    Article  CAS  Google Scholar 

  8. Benetti C, Angeletti R, Binato G, Biancardi A, Biamotto G (2008) Anal Chim Acta 617:132–138

    Article  CAS  Google Scholar 

  9. Allegrone G, Tamaro I, Spinardi S, Grosa G (2008) J Chromatogr A 1214:128–133

    Article  CAS  Google Scholar 

  10. Deng XJ, Guo DH, Li B, Zhu J, Yin P (2007) Chin J Chromatogr 25:39–42

    CAS  Google Scholar 

  11. Sun C, Chan SH, Lu D, Lee HMW, Bloodworth BC (2007) J Chromatogr A 1143:162–167

    Article  CAS  Google Scholar 

  12. Pico Y, Barcelo D (2008) Trac-Trends Anal Chem 27:821–835

    Article  CAS  Google Scholar 

  13. Wei J, Jin YZ (2005) UV curing coatings. Chemical Industry, Beijing

    Google Scholar 

  14. Rundlett KL, Armstrong DW (1996) Anal Chem 68:3493–3497

    Article  CAS  Google Scholar 

  15. Analytical Methods Committee (1994) Analyst 119:2363–2366

    Article  Google Scholar 

  16. D'Archivio AA, Fanelli M, Mazzeo P, Ruggieri F (2007) Talanta 71:25–30

    Article  Google Scholar 

  17. Rodil R, Quintana JB, Lopez-Mahia P, Muniategui-Lorenzo S, Prada-Rodriguez D (2009) J Chromatogr A 1216:2958–2969

    Article  CAS  Google Scholar 

  18. Ja XF, Shao B, Wu YN, Yang Y, Zhang J (2008) J AOAC Int 91:461–468

    Google Scholar 

  19. Di Gianni A, Bongiovanni R, Priola A, Turri S (2004) Int J Adhes Adhes 24:513–518

    Google Scholar 

  20. Rothenbacher T, Baumann M, Fügel D (2007) Food Addit Contam 24:438–444

    Article  CAS  Google Scholar 

  21. Gil-Vergara A, Blasco C, Pico Y (2007) Anal Bioanal Chem 389:605–617

    Article  CAS  Google Scholar 

  22. Sanches-Silva A, Pastorelli S, Cruz JM, Simoneau C, Castanheira I, Paseiro-Losada P (2008) J Agric Food Chem 56:2722–2726

    Article  CAS  Google Scholar 

  23. Sanches-Silva A, Pastorelli S, Cruz JM, Simoneau C, Paseiro-Losada P (2008) J Food Sci 73:C92–C99

    Article  CAS  Google Scholar 

Download references

Acknowledgments

This work was supported by National Basic Research Program of China (973 program, No. 2009CB421601), National Natural Science Fund of China (20575027, 90913012), National Science Funds for Creative Research Groups (20821063), National High-tech R&D Program (863 project, No. 2006AA10Z450), Science Foundation of Jiangsu (BM 2007511) and Analysis & Test Fund of Nanjing University.

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Authors and Affiliations

  1. Key Laboratory of Analytical Chemistry for Life Science (Ministry of Education of China), School of Chemistry & Chemical Engineering and Center of Materials Analysis, Nanjing University, 22 Hankou Road, Nanjing, 210093, China

    Dong-xu Shen & Hong-zhen Lian

  2. Jiangsu Entry–Exit Inspection and Quarantine Bureau of PRC, 99 Zhonghua Road, Nanjing, 210001, China

    Tao Ding, Jin-zhong Xu & Chong-yu Shen

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  1. Dong-xu Shen
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  2. Hong-zhen Lian
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  3. Tao Ding
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  4. Jin-zhong Xu
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  5. Chong-yu Shen
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Correspondence to Hong-zhen Lian or Chong-yu Shen.

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Shen, Dx., Lian, Hz., Ding, T. et al. Determination of low-level ink photoinitiator residues in packaged milk by solid-phase extraction and LC-ESI/MS/MS using triple-quadrupole mass analyzer. Anal Bioanal Chem 395, 2359–2370 (2009). https://doi.org/10.1007/s00216-009-3115-z

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