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. 2022 Jan 25;11(3):331.
doi: 10.3390/foods11030331.

Multiclass Comparative Analysis of Veterinary Drugs, Mycotoxins, and Pesticides in Bovine Milk by Ultrahigh-Performance Liquid Chromatography-Hybrid Quadrupole-Linear Ion Trap Mass Spectrometry

Qi Jia  1   2 , Jing Qiu  1   2 , Lin Zhang  1 , Guangqin Liao  1 , Yanbo Jia  3 , Yongzhong Qian  1   2
Affiliations

Multiclass Comparative Analysis of Veterinary Drugs, Mycotoxins, and Pesticides in Bovine Milk by Ultrahigh-Performance Liquid Chromatography-Hybrid Quadrupole-Linear Ion Trap Mass Spectrometry

Qi Jia et al. Foods. .

Abstract

A multiclass and multiresidue method for simultaneously screening and confirming veterinary drugs, mycotoxins, and pesticides in bovine milk was developed and validated with ultrahigh-performance liquid chromatography-hybrid quadrupole-linear ion trap mass spectrometry (UHPLC-Qtrap-MS). A total of 209 targeted contaminants were effectively extracted using an optimized QuEChERS method. Quantitative and qualitative confirmation were achieved simultaneously by multiple reaction monitoring-information-dependent acquisition-enhanced product ion (MRM-IDA-EPI) scan mode. The validation results exhibited a good sensitivity with the LOQs of 0.05-5 μg/kg, which was satisfactory for their MRLs in China or EU. The recoveries of in-house spiked samples were in the range of 51.20-129.76% with relative standard deviations (RSD) between replicates (n = 3) 0.82% and 19.76%. The test results of 140 milk samples from supermarkets and dairy farms in China showed that cloxacillin, aflatoxin M1, acetamiprid, and fipronil sulfone were found with lower concentrations. Combined with the residue results from the literature, penicillin G and cloxacillin (beta-lactams), enrofloxacin and ciprofloxacin (fluoroquinolones), and sulfamerazine (sulfonamides) were more frequently detected in different countries and need to receive more attention regarding their monitoring and control.

Keywords: liquid chromatography–triple qtrap mass spectrometry; milk; mycotoxin; pesticide; veterinary drug.

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Conflict of interest statement

Yanbo Jia is an employee of Shanghai AB Sciex Analytical Instrument Trading Company. The main work involved providing the data analysis method by the MRM-IDA-EPI mode. The authors have no influence on the correctness and objectivity of the conclusions of the manuscript. The authors declare no conflict of interest.

Figures

Figure 1
Figure 1
Comparison of ME values between 0.8 and 1.2 from the series of AA in ACN extraction solutions.
Figure 2
Figure 2
Comparison of ME values between 0.8 and 1.2 by extraction of 2% AA ACN and 2% FA ACN.
Figure 3
Figure 3
Comparison of recovery by different absorbents.
Figure 4
Figure 4
(a) Typical MRM chromatogram of aflatoxin M1 in bovine milk; (b) Product ion spectrums of aflatoxin M1 in bovine milk; (c) Product ion spectrums of aflatoxin M1 in standard product ion spectrums in database library.
See this image and copyright information in PMC

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