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Rapid determination of 48 stimulant residues in milk and dairy products by high-performance liquid chromatography coupled with quadrupole/Orbitrap high-resolution mass spectrometry

Yanjing Shi, Yali Zhang, Qiang He, Lu Zhang, and Meng Jin

Technology Centre of Xi’an Customs People’s Republic of China, Xi’an, China



Received: 10 November 2022  Accepted: 4 May 2023


A fast and easy method was proposed for the determination and quantification of 48 stimulants in milk and dairy products using high-performance liquid chromatography coupled with quadrupole/electrostatic field Orbitrap high-resolution mass spectrometry (Q Exactive). The samples were extracted with acetonitrile having 0.1% formic acid, and then, the extracting solution was purified using a Captive EMR-LIPID solid-phase extraction column. The main force between the target compound and the adsorbent was size exclusion. Unbranched long aliphatic chains on the lipids entered the sorbent, while bulky analytes did not, which could effectively remove the phosphorus esters in dairy products. Finally, we determined the instrument conditions. The samples were separated on a C18 column and eluted with acetonitrile and 0.05% formic acid aqueous solution as the mobile phases. Determination was then performed by mass spectrometry in electrospray ion source mode and monitored in parallel by reaction monitoring full scan/data-dependent secondary scan (Full MS/DD-MS2) mode. Under optimal conditions, the limit of quantification for the 48 stimulants was 0.5–100 µg L−1 in the milk and dairy products samples. The recoveries were 60.6–118.9% for milk, 63.2–123.8% for milk powder, and 61.8–119.6% for yogurt, with a determined coefficient of variation of less than 15%. The limit of detection values was 0.1–5.0 µg kg−1, and the limit of quantification values for the analytes was 0.2–10.0 µg kg−1. Finally, this method was used to screen 48 stimulants in 50 milk and dairy product samples.

Keywords: Q Exactive; Stimulants; Milk; Dairy products

Full paper is available at

DOI: 10.1007/s11696-023-02859-4


Chemical Papers 77 (9) 5237–5258 (2023)

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