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Rapid Confirmation Analysis of Multiple Antibiotic Residues in Honey by LC-MS/MS

Year 2023, Volume: 16 Issue: 4, 464 - 471, 31.12.2023

Nurullah Özdemir

https://doi.org/10.30607/kvj.1332421

Abstract

Honey is a natural product containing high levels of sugar, amino acids, minerals, enzymes and vitamins and has been used as food and medicine for thousands of years. In terms of public health, honey should not contain any chemicals that may pose a health risk. Both pesticides used in agricultural areas around the apiary and drugs used in the treatment of bee diseases cause residue problems in honey. In the study, it was aimed to develop a method for rapid confirmation analysis of multiple antibiotic residues in honey samples using a two-stage liquid-liquid extraction method. With the developed method, sulphonamide (n:11), fluoroquinolone (n:2), phenicol (n:2) tetracycline (n:2) and macrolide (n:2) were used in honey samples. Screening and confirmation analyses can be performed for 19 antibiotic residues in 5 different antibiotic groups. The detection limits of the method are between 5.29 and 10.58 µg.kg-1, the accuracy values are between 86.9% and 119%, the coefficient of variation is between 1.26% and 16.33% and recovery is between 84% and 117.23%.

Keywords

Antibiotic Confirmation Honey LC-MS/MS Residue

References

  • Ball, D.W. (2007). The chemical composition of honey Journal of Chemical Education, 84(10), 1643. https://pubs.acs.org/doi/abs/10.1021/ed084p1643
  • Bargańska, Ż., Namieśnik, J., & Ślebioda, M. (2011). Determination of antibiotic residues in honey. TrAC Trends in Analytical Chemistry, 30(7), 1035-1041. https://doi.org/10.1016/j.trac.2011.02.014
  • Commission Regulation (CR). (2010). No 37/2010 of 22 December 2009. Official Journal of the European Communities. 2010; L15: 1–72. doi:10.3000/17252555.L_2010.015.eng [Erişim Tarihi:22.07.2023]. https://eur-lex.europa.eu/legal-content/EN/TXT/HTML/?uri=OJ:L:2010:175:FULL&from=SL
  • Community Reference Laboratories (CRL). (2007). Guidance Paper, CRLs view on state of the art analytical methods for national residue control plans (7 December 2007). [Erişim Tarihi:22.07.2023]. http://www.media-bank.co.kr/board_data/Erythromycin%20CRL%20guidance%202007.pdf
  • Chantawannakul, P., de Guzman, L.I., Li, J., & Williams, G.R. Parasites, pathogens, and pests of honeybees in Asia. Apidologie 47, 301–324 (2016). https://doi.org/10.1007/s13592-015-0407-5
  • Chen, H., Chen, H., Ying, J., Huang, J., & Liao, L. (2009). Dispersive liquid–liquid microextraction followed by high-performance liquid chromatography as an efficient and sensitive technique for simultaneous determination of chloramphenicol and thiamphenicol in honey. Analytica chimica acta, 632(1), 80-85. https://doi.org/10.1016/j.aca.2008.10.068
  • Chiesa, L. M., Panseri, S., Nobile, M., Ceriani, F., & Arioli, F. (2018). Distribution of POPs, pesticides and antibiotic residues in organic honeys from different production areas. Food Additives & Contaminants: Part A, 35(7), 1340-1355. https://www.tandfonline.com/doi/epdf/10.1080/19440049.2018.1451660?needAccess=true&role=button
  • El Hawari, K., Mokh, S., Doumyati, S., Al Iskandarani, M., & Verdon, E. (2017). Development and validation of a multiclass method for the determination of antibiotic residues in honey using liquid chromatography-tandem mass spectrometry. Food Additives & Contaminants: Part A,34(4),582-597. https://www.tandfonline.com/doi/epdf/10.1080/19440049.2016.1232491?needAccess=true&role=button
  • Kivrak, I., KIVRAK, Ş., & Harmandar, M. (2016). Development of a rapid method for the determination of antibiotic residues in honey using UPLC-ESI-MS/MS. Food Science and Technology, 36, 90-96. https://www.scielo.br/j/cta/a/GqkpZ8mXfNpPhZ3JXqDS5Ls/
  • Lambert, O., Piroux, M., Puyo, S., Thorin, C., L'Hostis, M., Wiest, L., ... & Pouliquen, H. (2013). Widespread occurrence of chemical residues in beehive matrices from apiaries located in different landscapes of Western France. PloS one,8(6),e67007. https://journals.plos.org/plosone/article?id=10.1371/journal.pone.0067007
  • Lopez, M. I., Pettis, J. S., Smith, I. B., & Chu, P. S. (2008). Multiclass determination and confirmation of antibiotic residues in honey using LC-MS/MS. Journal of Agricultural and Food Chemistry, 56(5), 1553-1559. https://pubs.acs.org/doi/abs/10.1021/jf073236w
  • Louppis, A.P., Kontominas, M. G., & Papastephanou, C. (2017). Determination of antibiotic residues in honey by high-performance liquid chromatography with electronspray ionization tandem mass spectrometry. Food Analytical Methods, 10, 3385-3397. https://link.springer.com/article/10.1007/s12161-017-0899-x
  • Mahmoudi, R., Norian, R., & Pajohi-Alamoti, M. (2014). Antibiotic residues in Iranian honey by ELISA. International journal of food properties, 17(10), 2367-2373.
  • Moretti, S., Saluti, G., & Galarini, R. (2017). Residue Determination in Honey. InTech. doi: 10.5772/67135 https://academic.oup.com/jaoac/article/92/3/975/5655938?login=false
  • Peres, G. T., Rath, S., & Reyes, F. G. R. (2010). A HPLC with fluorescence detection method for the determination of tetracyclines residues and evaluation of their stability in honey. Food control, 21(5), 620-625.
  • Resmî Gazete. (2017). 07.03.2017 Tarih ve 30000 sayılı. Türk Gıda Kodeksi Hayvansal Gıdalarda Bulunabilecek Farmakolojik Aktif Maddelerin Sınıflandırılması ve Maksimum Kalıntı Limitleri Yönetmeliği. [Erişim Tarihi:22.07.2023].https://www.resmigazete.gov.tr/eskiler/2017/03/20170307-4.htm
  • Reybroeck, W., Daeseleire, E., De Brabander, H. F., & Herman, L. (2012). Antimicrobials in beekeeping. Veterinary microbiology, 158(1-2), 1-11. https://www.sciencedirect.com/science/article/pii/S0378113512000326
  • Salter, R. (2003). Charm II system-comprehensive residue analysis system for honey. Apiacta, 38, 198-206. http://charmdev-websitetestlink.charm.com/wp-content/uploads/2018/06/EX-0162.pdf
  • Varenina, I., Bilandžić, N., Luburić, Đ. B., Kolanović, B. S., Varga, I., Sedak, M., & Đokić, M. (2023). Determination of quinolones, macrolides, sulfonamides and tetracyclines in honey using QuEChERS sample preparation and UHPLC-MS/MS analysis. Food Control, 148,109676. https://doi.org/10.1016/j.foodcont.2023.109676
  • Vidal, J. L. M., Aguilera-Luiz, M. D. M., Romero-Gonzalez, R., & Frenich, A. G. (2009). Multiclass analysis of antibiotic residues in honey by ultraperformance liquid chromatography− tandem mass spectrometry. Journal of agricultural and food chemistry, 57(5), 1760-1767. https://pubs.acs.org/doi/abs/10.1021/jf8034572
  • Wutz, K., Niessner, R., & Seidel, M. (2011). Simultaneous determination of four different antibiotic residues in honey by chemiluminescence multianalyte chip immunoassays. Microchimica Acta, 173, 1-9. https://link.springer.com/article/10.1007/s00604-011-0548-9
  • Xu, J. J., An, M., Yang, R., Tan, Z., Hao, J., Cao, J., & Cao, W. (2016). Determination of tetracycline antibiotic residues in honey and milk by miniaturized solid phase extraction using chitosan-modified graphitized multiwalled carbon nanotubes. Journal of Agricultural and Food Chemistry, 64(12), 2647-2654. https://pubs.acs.org/doi/abs/10.1021/acs.jafc.6b00748
  • Yang, Y., Lin, G., Liu, L., & Lin, T. (2022). Rapid determination of multi-antibiotic residues in honey based on modified QuEChERS method coupled with UPLC–MS/MS. Food Chemistry, 374, 131733. https://doi.org/10.1016/j.foodchem.2021.131733

Balda Çoklu Antibiyotik Kalıntılarının LC-MS/MS ile Hızlı Doğrulama Analizi

Year 2023, Volume: 16 Issue: 4, 464 - 471, 31.12.2023

Nurullah Özdemir

https://doi.org/10.30607/kvj.1332421

Abstract

Bal, yüksek oranda şeker, aminoasit, mineral madde, enzim ve vitamin içeren, binlerce yıldır gıda ve ilaç olarak kullanılan doğal bir üründür. Halk sağlığı açısından, balda sağlık riski oluşturabilecek herhangi bir kimyasal maddenin bulunmaması gerekir. Gerek arılık çevresindeki tarımsal alanlarda kullanılan pestisitler, gerekse arı hastalıklarının tedavisinde kullanılan ilaçlar, bal da kalıntı sorunlarının yaşanmasına neden olmaktadır. Çalışmada, iki farklı likit-likit ekstraksiyon metodu kullanılarak bal örneklerinde çoklu antibiyotik kalıntılarının hızlı doğrulama analizleri için metot geliştirilmesi amaçlanmıştır. Geliştirilen metotla, bal örneklerinde, sulfonamid (n:11), flourokinolon (n:2), fenikol (n:2) tetrasiklin (n:2) ve makrolid (n:2) olmak üzere 5 farklı antibiyotik grubunda 19 adet antibiyotik kalıntısı için tarama ve doğrulama analizleri yapılabilir. Metodun tespit limitleri 5,29 ile 10,58 µg.kg-1, doğruluk değerleri %86,9 ile %119 varyasyon katsayı değerleri %1,26 ile %16,33 ve geri kazanım oranları %85,4 ile %117,23 arasındadır.

Keywords

Antibiyotik Bal Doğrulama Kalıntı LC-MS/MS

References

  • Ball, D.W. (2007). The chemical composition of honey Journal of Chemical Education, 84(10), 1643. https://pubs.acs.org/doi/abs/10.1021/ed084p1643
  • Bargańska, Ż., Namieśnik, J., & Ślebioda, M. (2011). Determination of antibiotic residues in honey. TrAC Trends in Analytical Chemistry, 30(7), 1035-1041. https://doi.org/10.1016/j.trac.2011.02.014
  • Commission Regulation (CR). (2010). No 37/2010 of 22 December 2009. Official Journal of the European Communities. 2010; L15: 1–72. doi:10.3000/17252555.L_2010.015.eng [Erişim Tarihi:22.07.2023]. https://eur-lex.europa.eu/legal-content/EN/TXT/HTML/?uri=OJ:L:2010:175:FULL&from=SL
  • Community Reference Laboratories (CRL). (2007). Guidance Paper, CRLs view on state of the art analytical methods for national residue control plans (7 December 2007). [Erişim Tarihi:22.07.2023]. http://www.media-bank.co.kr/board_data/Erythromycin%20CRL%20guidance%202007.pdf
  • Chantawannakul, P., de Guzman, L.I., Li, J., & Williams, G.R. Parasites, pathogens, and pests of honeybees in Asia. Apidologie 47, 301–324 (2016). https://doi.org/10.1007/s13592-015-0407-5
  • Chen, H., Chen, H., Ying, J., Huang, J., & Liao, L. (2009). Dispersive liquid–liquid microextraction followed by high-performance liquid chromatography as an efficient and sensitive technique for simultaneous determination of chloramphenicol and thiamphenicol in honey. Analytica chimica acta, 632(1), 80-85. https://doi.org/10.1016/j.aca.2008.10.068
  • Chiesa, L. M., Panseri, S., Nobile, M., Ceriani, F., & Arioli, F. (2018). Distribution of POPs, pesticides and antibiotic residues in organic honeys from different production areas. Food Additives & Contaminants: Part A, 35(7), 1340-1355. https://www.tandfonline.com/doi/epdf/10.1080/19440049.2018.1451660?needAccess=true&role=button
  • El Hawari, K., Mokh, S., Doumyati, S., Al Iskandarani, M., & Verdon, E. (2017). Development and validation of a multiclass method for the determination of antibiotic residues in honey using liquid chromatography-tandem mass spectrometry. Food Additives & Contaminants: Part A,34(4),582-597. https://www.tandfonline.com/doi/epdf/10.1080/19440049.2016.1232491?needAccess=true&role=button
  • Kivrak, I., KIVRAK, Ş., & Harmandar, M. (2016). Development of a rapid method for the determination of antibiotic residues in honey using UPLC-ESI-MS/MS. Food Science and Technology, 36, 90-96. https://www.scielo.br/j/cta/a/GqkpZ8mXfNpPhZ3JXqDS5Ls/
  • Lambert, O., Piroux, M., Puyo, S., Thorin, C., L'Hostis, M., Wiest, L., ... & Pouliquen, H. (2013). Widespread occurrence of chemical residues in beehive matrices from apiaries located in different landscapes of Western France. PloS one,8(6),e67007. https://journals.plos.org/plosone/article?id=10.1371/journal.pone.0067007
  • Lopez, M. I., Pettis, J. S., Smith, I. B., & Chu, P. S. (2008). Multiclass determination and confirmation of antibiotic residues in honey using LC-MS/MS. Journal of Agricultural and Food Chemistry, 56(5), 1553-1559. https://pubs.acs.org/doi/abs/10.1021/jf073236w
  • Louppis, A.P., Kontominas, M. G., & Papastephanou, C. (2017). Determination of antibiotic residues in honey by high-performance liquid chromatography with electronspray ionization tandem mass spectrometry. Food Analytical Methods, 10, 3385-3397. https://link.springer.com/article/10.1007/s12161-017-0899-x
  • Mahmoudi, R., Norian, R., & Pajohi-Alamoti, M. (2014). Antibiotic residues in Iranian honey by ELISA. International journal of food properties, 17(10), 2367-2373.
  • Moretti, S., Saluti, G., & Galarini, R. (2017). Residue Determination in Honey. InTech. doi: 10.5772/67135 https://academic.oup.com/jaoac/article/92/3/975/5655938?login=false
  • Peres, G. T., Rath, S., & Reyes, F. G. R. (2010). A HPLC with fluorescence detection method for the determination of tetracyclines residues and evaluation of their stability in honey. Food control, 21(5), 620-625.
  • Resmî Gazete. (2017). 07.03.2017 Tarih ve 30000 sayılı. Türk Gıda Kodeksi Hayvansal Gıdalarda Bulunabilecek Farmakolojik Aktif Maddelerin Sınıflandırılması ve Maksimum Kalıntı Limitleri Yönetmeliği. [Erişim Tarihi:22.07.2023].https://www.resmigazete.gov.tr/eskiler/2017/03/20170307-4.htm
  • Reybroeck, W., Daeseleire, E., De Brabander, H. F., & Herman, L. (2012). Antimicrobials in beekeeping. Veterinary microbiology, 158(1-2), 1-11. https://www.sciencedirect.com/science/article/pii/S0378113512000326
  • Salter, R. (2003). Charm II system-comprehensive residue analysis system for honey. Apiacta, 38, 198-206. http://charmdev-websitetestlink.charm.com/wp-content/uploads/2018/06/EX-0162.pdf
  • Varenina, I., Bilandžić, N., Luburić, Đ. B., Kolanović, B. S., Varga, I., Sedak, M., & Đokić, M. (2023). Determination of quinolones, macrolides, sulfonamides and tetracyclines in honey using QuEChERS sample preparation and UHPLC-MS/MS analysis. Food Control, 148,109676. https://doi.org/10.1016/j.foodcont.2023.109676
  • Vidal, J. L. M., Aguilera-Luiz, M. D. M., Romero-Gonzalez, R., & Frenich, A. G. (2009). Multiclass analysis of antibiotic residues in honey by ultraperformance liquid chromatography− tandem mass spectrometry. Journal of agricultural and food chemistry, 57(5), 1760-1767. https://pubs.acs.org/doi/abs/10.1021/jf8034572
  • Wutz, K., Niessner, R., & Seidel, M. (2011). Simultaneous determination of four different antibiotic residues in honey by chemiluminescence multianalyte chip immunoassays. Microchimica Acta, 173, 1-9. https://link.springer.com/article/10.1007/s00604-011-0548-9
  • Xu, J. J., An, M., Yang, R., Tan, Z., Hao, J., Cao, J., & Cao, W. (2016). Determination of tetracycline antibiotic residues in honey and milk by miniaturized solid phase extraction using chitosan-modified graphitized multiwalled carbon nanotubes. Journal of Agricultural and Food Chemistry, 64(12), 2647-2654. https://pubs.acs.org/doi/abs/10.1021/acs.jafc.6b00748
  • Yang, Y., Lin, G., Liu, L., & Lin, T. (2022). Rapid determination of multi-antibiotic residues in honey based on modified QuEChERS method coupled with UPLC–MS/MS. Food Chemistry, 374, 131733. https://doi.org/10.1016/j.foodchem.2021.131733
There are 23 citations in total.

Details

Primary Language Turkish
Subjects Veterinary Pharmacology
Journal Section RESEARCH ARTICLE
Authors

Nurullah Özdemir 0000-0003-4310-2077

Early Pub Date December 20, 2023
Publication Date December 31, 2023
Acceptance Date September 29, 2023
Published in Issue Year 2023 Volume: 16 Issue: 4

Cite

APA Özdemir, N. (2023). Balda Çoklu Antibiyotik Kalıntılarının LC-MS/MS ile Hızlı Doğrulama Analizi. Kocatepe Veterinary Journal, 16(4), 464-471. https://doi.org/10.30607/kvj.1332421
AMA Özdemir N. Balda Çoklu Antibiyotik Kalıntılarının LC-MS/MS ile Hızlı Doğrulama Analizi. kvj. December 2023;16(4):464-471. doi:10.30607/kvj.1332421
Chicago Özdemir, Nurullah. “Balda Çoklu Antibiyotik Kalıntılarının LC-MS/MS Ile Hızlı Doğrulama Analizi”. Kocatepe Veterinary Journal 16, no. 4 (December 2023): 464-71. https://doi.org/10.30607/kvj.1332421.
EndNote Özdemir N (December 1, 2023) Balda Çoklu Antibiyotik Kalıntılarının LC-MS/MS ile Hızlı Doğrulama Analizi. Kocatepe Veterinary Journal 16 4 464–471.
IEEE N. Özdemir, “Balda Çoklu Antibiyotik Kalıntılarının LC-MS/MS ile Hızlı Doğrulama Analizi”, kvj, vol. 16, no. 4, pp. 464–471, 2023, doi: 10.30607/kvj.1332421.
ISNAD Özdemir, Nurullah. “Balda Çoklu Antibiyotik Kalıntılarının LC-MS/MS Ile Hızlı Doğrulama Analizi”. Kocatepe Veterinary Journal 16/4 (December 2023), 464-471. https://doi.org/10.30607/kvj.1332421.
JAMA Özdemir N. Balda Çoklu Antibiyotik Kalıntılarının LC-MS/MS ile Hızlı Doğrulama Analizi. kvj. 2023;16:464–471.
MLA Özdemir, Nurullah. “Balda Çoklu Antibiyotik Kalıntılarının LC-MS/MS Ile Hızlı Doğrulama Analizi”. Kocatepe Veterinary Journal, vol. 16, no. 4, 2023, pp. 464-71, doi:10.30607/kvj.1332421.
Vancouver Özdemir N. Balda Çoklu Antibiyotik Kalıntılarının LC-MS/MS ile Hızlı Doğrulama Analizi. kvj. 2023;16(4):464-71.
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