Skip to main content
Log in

High-Throughput Determination of 30 Veterinary Drug Residues in Milk Powder by Dispersive Solid-Phase Extraction Coupled with Ultra-High Performance Liquid Chromatography Tandem Mass Spectrometry

  • Published:
Food Analytical Methods Aims and scope Submit manuscript

Abstract

A high-throughput method was established for the simultaneous determination of 30 β-agonists, fluoroquinolones, and cephalosporins in milk powder by dispersive solid-phase extraction (dSPE) and ultra-high performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS). Samples were firstly dissolved in sodium acetate buffer, then extracted with formic acid-acetonitrile, and subsequently purified by dSPE. Thirty target analytes were separated on a C18 column by gradient elution, detected through electrospray ionization (ESI) source in the positive mode with multi-reaction monitoring (MRM) conditions. The developed method was validated in terms of linearity, accuracy, and precision. Results indicated that 30 target analytes displayed excellent linearity in their corresponding concentration ranges and that their correlation coefficients were all higher than 0.995. The limits of quantitation (LOQs) for these targets were in the range of 0.7–7.0 μg/kg. The mean recoveries for negative sample spiked at three concentration levels were calculated between 80.0 and 97.5% with the relative standard deviation (RSD, n = 6) values ranging from 2.8 to 10.8%. In addition, the inter-day precision (n = 5) of the second spiked concentration was less than 13% (4.4–12.4%). The established and validated method is accurate and rapid and suitable for the high-throughput analysis of β-agonist, fluoroquinolone, and cephalosporin multi-residues in milk powder.

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

Access this article

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

Instant access to the full article PDF.

Fig. 1
Fig. 2
Fig. 3

Similar content being viewed by others

References

  • Anastassiades M, Lehotay SJ, Štajnbaher 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(2):412–431

    CAS  Google Scholar 

  • Aufartová J, Brabcová I, Torres-Padrón ME, Solich P, Sosa-Ferrera Z, Santana-Rodríguez JJ (2017) Determination of fluoroquinolones in fishes using microwave-assisted extraction combined with ultra-high performance liquid chromatography and fluorescence detection. J Food Compos Anal 56:140–146

    Article  Google Scholar 

  • Bousova K, Senyuva H, Mittendorf K (2013) Quantitative multi-residue method for determination antibiotics in chicken meat using turbulent flow chromatography coupled to liquid chromatography–tandem mass spectrometry. J Chromatogr A 1274:19–27

    Article  CAS  Google Scholar 

  • Chen D, Yu J, Tao Y, Pan Y, Xie S, Huang L, Peng D, Wang X, Wang Y, Liu Z, Yuan Z (2016) Qualitative screening of veterinary anti-microbial agents in tissues, milk, and eggs of food-producing animals using liquid chromatography coupled with tandem mass spectrometry. Journal of chromatography. B, Analytical technologies in the biomedical and life sciences 1017-1018:82–88

    Article  CAS  Google Scholar 

  • Chiesa L, Nobile M, Arioli F, Britti D, Trutic N, Pavlovic R, Panseri S (2015) Determination of veterinary antibiotics in bovine urine by liquid chromatography–tandem mass spectrometry. Food Chem 185:7–15

    Article  CAS  Google Scholar 

  • Chu L, Zheng S, Qu B, Geng S, Kang X (2017) Detection of β-agonists in pork tissue with novel electrospun nanofibers-based solid-phase extraction followed ultra-high performance liquid chromatography/tandem mass spectrometry. Food Chem 227:315–321

    Article  CAS  Google Scholar 

  • Dang H, Liu D, Hou X, Wu Y, Wang B, Dong H, Xian Y (2017) One-step extraction prior to two-step detection by ultra high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) to determine different groups of antibacterial agents in infant disposable hygiene products. Anal Methods 9(3):482–489

    Article  CAS  Google Scholar 

  • Dasenaki ME, Thomaidis NS (2015) Multi-residue determination of 115 veterinary drugs and pharmaceutical residues in milk powder, butter, fish tissue and eggs using liquid chromatography–tandem mass spectrometry. Anal Chim Acta 880:103–121

    Article  CAS  Google Scholar 

  • de Oliveira HL, da Silva Anacleto S, da Silva ATM, Pereira AC, de Souza Borges W, Figueiredo EC, Borges KB (2016) Molecularly imprinted pipette-tip solid phase extraction for selective determination of fluoroquinolones in human urine using HPLC-DAD. J Chromatogr B 1033–1034:27–39

    Article  Google Scholar 

  • Denadai M, Cass QB (2015) Simultaneous determination of fluoroquinolones in environmental water by liquid chromatography–tandem mass spectrometry with direct injection: a green approach. J Chromatogr A 1418:177–184

    Article  CAS  Google Scholar 

  • Dong H, Guo X, Xian Y, Luo H, Wang B, Wu Y (2015) A salting out-acetonitrile homogeneous extraction coupled with gas chromatography–mass spectrometry method for the simultaneous determination of thirteen N-nitrosamines in skin care cosmetics. J Chromatogr A 1422:82–88

    Article  CAS  Google Scholar 

  • Dong H, Luo D, Xian Y, Luo H, Guo X, Li C, Zhao M (2016) Adulteration identification of commercial honey with the C-4 sugar content of negative values by an elemental analyzer and liquid chromatography coupled to isotope ratio mass spectroscopy. J Agric Food Chem 64(16):3258–3265

    Article  CAS  Google Scholar 

  • Dong H, Xiao K (2017) Modified QuEChERS combined with ultra high performance liquid chromatography tandem mass spectrometry to determine seven biogenic amines in Chinese traditional condiment soy sauce. Food Chem 229:502–508

    Article  CAS  Google Scholar 

  • Guo X, Mu T, Xian Y, Luo D, Wang C (2016) Ultra-performance liquid chromatography tandem mass spectrometry for the rapid simultaneous analysis of nine organophosphate esters in milk powder. Food Chem 196:673–681

    Article  CAS  Google Scholar 

  • Jia W, Chu X, Chang J, Wang PG, Chen Y, Zhang F (2017) High-throughput untargeted screening of veterinary drug residues and metabolites in tilapia using high resolution orbitrap mass spectrometry. Anal Chim Acta 957:29–39

    Article  CAS  Google Scholar 

  • Jin Y, Zhang J, Zhao W, Zhang W, Wang L, Zhou J, Li Y (2017) Development and validation of a multiclass method for the quantification of veterinary drug residues in honey and royal jelly by liquid chromatography–tandem mass spectrometry. Food Chem 221:1298–1307

    Article  CAS  Google Scholar 

  • Khezeli T, Daneshfar A (2017) Development of dispersive micro-solid phase extraction based on micro and nano sorbents. TrAC Trends Anal Chem 89:99–118

    Article  CAS  Google Scholar 

  • Li W, Shen H, Hong Y, Zhang Y, Yuan F, Zhang F (2016) Simultaneous determination of 22 cephalosporins drug residues in pork muscle using liquid chromatography–tandem mass spectrometry. J Chromatogr B 1022:298–307

    Article  CAS  Google Scholar 

  • Liu X, Yu Y, Zhao M, Zhang H, Li Y, Duan G (2014) Solid phase extraction using magnetic core mesoporous shell microspheres with C18-modified interior pore-walls for residue analysis of cephalosporins in milk by LC–MS/MS. Food Chem 150:206–212

    Article  CAS  Google Scholar 

  • Luo D, Dong H, Luo H, Xian Y, Guo X, Wu Y (2016) Multi-element (C, N, H, O) stable isotope ratio analysis for determining the geographical origin of pure milk from different regions. Food Anal Methods 9(2):437–442

    Article  Google Scholar 

  • Luo D, Dong H, Luo H, Xian Y, Wan J, Guo X, Wu Y (2015) The application of stable isotope ratio analysis to determine the geographical origin of wheat. Food Chem 174:197–201

    Article  CAS  Google Scholar 

  • Masiá A, Suarez-Varela MM, Llopis-Gonzalez A, Picó Y (2016) Determination of pesticides and veterinary drug residues in food by liquid chromatography-mass spectrometry: a review. Anal Chim Acta 936:40–61

    Article  Google Scholar 

  • Matuszewski BK, Chavez-Eng CM (2003) Strategies for the assessment of matrix effect in quantitative bioanalytical methods based on HPLC-MS/MS. Anal Chem 75(13):3019–3030

    Article  CAS  Google Scholar 

  • Mauro D, Ciardullo S, Civitareale C, Fiori M, Pastorelli AA, Stacchini P, Palleschi G (2014) Development and validation of a multi-residue method for determination of 18 β-agonists in bovine urine by UPLC–MS/MS. Microchem J 115:70–77

    Article  CAS  Google Scholar 

  • Rico A, Van den Brink PJ (2014) Probabilistic risk assessment of veterinary medicines applied to four major aquaculture species produced in Asia. Sci Total Environ 468–469:630–641

    Article  Google Scholar 

  • Wang P, Liu X, Su X, Zhu R (2015) Sensitive detection of β-agonists in pork tissue with novel molecularly imprinted polymer extraction followed liquid chromatography coupled tandem mass spectrometry detection. Food Chem 184:72–79

    Article  CAS  Google Scholar 

  • Wu Y, Luo D, Dong H, Wan J, Luo H, Xian Y, Guo X, Qin F, Han W, Wang L, Wang B (2015) Geographical origin of cereal grains based on element analyser-stable isotope ratio mass spectrometry (EA-SIRMS). Food Chem 174:553–557

    Article  CAS  Google Scholar 

  • Wu Z, Xu Y, Li M, Guo X, Xian Y, Dong H (2016a) Determination of three fluorescent whitening agents (FWAs) and their migration research in food contact plastic packaging containers and food simulants by UPLC-MS/MS method. RSC Adv 6(22):17941–17946

    Article  CAS  Google Scholar 

  • Wu Z, Xu Y, Li M, Guo X, Xian Y, Dong H (2016b) Simultaneous determination of fluorescent whitening agents (FWAs) and photoinitiators (PIs) in food packaging coated paper products by the UPLC-MS/MS method using ESI positive and negative switching modes. Anal Methods 8(5):1052–1059

    Article  CAS  Google Scholar 

  • Xian Y, Dong H, Wu Y, Guo X, Hou X, Wang B (2016) QuEChERS-based purification method coupled to ultrahigh performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) to determine six quaternary ammonium compounds (QACs) in dairy products. Food Chem 212:96–103

    Article  CAS  Google Scholar 

  • Yang Y, Shao B, Zhang J, Wu Y, Duan H (2009) Determination of the residues of 50 anabolic hormones in muscle, milk and liver by very-high-pressure liquid chromatography–electrospray ionization tandem mass spectrometry. J Chromatogr B 877(5–6):489–496

    Article  CAS  Google Scholar 

  • Zeng X, Bai W, Xian Y, Dong H, Luo D (2016) Application of QuEChERS-based purification coupled with isotope dilution gas chromatography-mass spectrometry method for the determination of N-nitrosamines in soy sauce. Anal Methods 8(26):5248–5254

    Article  CAS  Google Scholar 

  • Zhan J, Zhong YY, Yu XJ, Peng JF, Chen S, Yin JY, Zhang JJ, Zhu Y (2013) Multi-class method for determination of veterinary drug residues and other contaminants in infant formula by ultra performance liquid chromatography–tandem mass spectrometry. Food Chem 138(2–3):827–834

    Article  CAS  Google Scholar 

  • Zhu WX, Yang JZ, Wang Z-X, Wang CJ, Liu YF, Zhang L (2016) Rapid determination of 88 veterinary drug residues in milk using automated TurborFlow online clean-up mode coupled to liquid chromatography-tandem mass spectrometry. Talanta 148:401–411

    Article  CAS  Google Scholar 

Download references

Author information

Authors and Affiliations

Authors

Corresponding authors

Correspondence to Ruijiao Li or Moucheng Wu.

Ethics declarations

Conflict of Interest

Ruijiao Li declares that she has no conflict of interest. Moucheng Wu declares that he has no conflict of interest.

Ethical Approval

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

Informed Consent

Not applicable.

Rights and permissions

Reprints and permissions

About this article

Check for updates. Verify currency and authenticity via CrossMark

Cite this article

Li, R., Wu, M. High-Throughput Determination of 30 Veterinary Drug Residues in Milk Powder by Dispersive Solid-Phase Extraction Coupled with Ultra-High Performance Liquid Chromatography Tandem Mass Spectrometry. Food Anal. Methods 10, 3753–3762 (2017). https://doi.org/10.1007/s12161-017-0941-z

Download citation

  • Received:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s12161-017-0941-z

Keywords

Navigation