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Rapid Screening and Determination of the Residues of Hormones and Sedatives in Milk Powder Using the UHPLC-MS/MS and SPE

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Abstract

A method based on the ultra-high-performance liquid chromatography tandem mass spectrometry for determination of the residues of sex hormones, glucocorticoids, and sedatives in milk powder was developed. The sample was extracted with the acetic acid-acetonitrile (1:99, v/v) twice, purified by the PRiME hydrophilic-lipophilic balance (HLB) cartridges and analyzed by the ultra-high-performance liquid chromatography-tandem mass spectrometry. The analytes were separated by the Waters Acquity UPLC™ BEH C18 column (50 mm × 2.1 mm, 1.7 μm) and determined using the electrospray ionization in the positive mode with the multiple reaction monitoring (MRM). The developed method was validated with the specificity, linearity and range, matrix effects, recovery, and precision. The results showed that the analytes were linear with the correlation of determinations (R2) higher than 0.991 in the corresponding ranges. The limits of detection (LODs) and limits of quantification (LOQs) were in the range of 0.1–1.1 μg kg−1 and 0.3–3.8 μg kg−1, respectively. The average recoveries of the analytes ranged from 78.5 to 107.0% with the relative standard deviations lower than 15%. The practical applicability was tested by analyzing real samples and the progesterone was observed in two samples.

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Authors and Affiliations

  1. College of Pharmacy, Chongqing Medical University, Chongqing, 400016, China

    Jia Zheng & Zhaode Mu

  2. Chongqing Key Laboratory of Biochemistry and Molecular Pharmacology, Chongqing, 400016, China

    Jia Zheng & Zhaode Mu

  3. Chongqing Entry–Exit Inspection and Quarantine Bureau, Chongqing, 400020, China

    Cunxian Xi, Guomin Wang, Shurui Cao & Bobin Tang

  4. Chongqing Engineering Technology Research Center of Import and Export Food Safety, Chongqing, 400020, China

    Cunxian Xi, Guomin Wang, Shurui Cao & Bobin Tang

Authors
  1. Jia Zheng
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  2. Cunxian Xi
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  3. Guomin Wang
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  4. Shurui Cao
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  5. Bobin Tang
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  6. Zhaode Mu
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Correspondence to Zhaode Mu.

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Conflict of Interest

Jia Zheng declares that she has no conflict of interest. Cunxian Xi declares that he has no conflict of interest. Shurui Cao declares that she has no conflict of interest. Guomin Wang declares that he has no conflict of interest. Bobin Tang declares that he has no conflict of interest. Zhaode Mu declares that she has no conflict of interest.

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

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Informed consent was obtained from all individual participants included in the study.

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Zheng, J., Xi, C., Wang, G. et al. Rapid Screening and Determination of the Residues of Hormones and Sedatives in Milk Powder Using the UHPLC-MS/MS and SPE. Food Anal. Methods 11, 3435–3451 (2018). https://doi.org/10.1007/s12161-018-1317-8

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  • DOI: https://doi.org/10.1007/s12161-018-1317-8

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