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. 2023 Dec 22;29(1):96.
doi: 10.3390/molecules29010096.

Simultaneous Determination of Steroids and NSAIDs, Using DLLME-SFO Extraction and HPLC Analysis, in Milk and Eggs Collected from Rural Roma Communities in Transylvania, Romania

Mihaela Cătălina Herghelegiu  1 , Vlad Alexandru Pănescu  1 , Victor Bocoș-Bințințan  1 , Radu-Tudor Coman  2 , Vidar Berg  3 , Jan Ludvig Lyche  3 , Maria Concetta Bruzzoniti  4 , Mihail Simion Beldean-Galea  1
Affiliations

Simultaneous Determination of Steroids and NSAIDs, Using DLLME-SFO Extraction and HPLC Analysis, in Milk and Eggs Collected from Rural Roma Communities in Transylvania, Romania

Mihaela Cătălina Herghelegiu et al. Molecules. .

Abstract

This research aims to determine five steroids and four non-steroidal anti-inflammatory drugs in milk and egg samples collected from rural Roma communities in Transylvania, Romania. Target compounds were extracted from selected matrices by protein precipitation, followed by extract purification by dispersive liquid-liquid microextraction based on solidification of floating organic droplets. The extraction procedure was optimized using a 24 full factorial experimental design. Good enrichment factors (87.64-122.07 milk; 26.97-38.72 eggs), extraction recovery (74.49-103.76% milk; 75.64-108.60% eggs), and clean-up of the sample were obtained. The method detection limits were 0.74-1.77 µg/L for milk and 2.39-6.02 µg/kg for eggs, while the method quantification limits were 2.29-5.46 µg/L for milk and 7.38-18.65 µg/kg for eggs. The steroid concentration in milk samples was <MDL up to 4.30 µg/L, decreasing from 17α-ethinyl estradiol, 17β-estradiol, and estrone to estriol. The NSAID concentration was <MDL up to 3.41 µg/L, decreasing from ibuprofen, diclofenac, and ketoprofen to naproxen. The steroid concentration in the egg samples was <MDL to 2.79 µg/kg, with all steroids detected, while the concentration of NSAIDs was <MDL to 2.28 µg/kg, with only ibuprofen, ketoprofen, and naproxen detected. The developed protocol was successfully applied to the analysis of target compounds in real milk and egg samples.

Keywords: dispersive liquid–liquid microextraction based on solidification of floating organic droplets (DLLME-SFO); eggs; milk; non-steroidal anti-inflammatory drugs (NSAIDs); rural Roma communities; steroids.

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Conflict of interest statement

The authors declare no conflict of interest.

Figures

Figure 1
Figure 1
Chromatograms obtained at 190 nm of milk sample ((A) black color) and spiked milk sample with 100 ng of each compound ((A) green color). Chromatograms of egg sample ((B) black color) and spiked egg sample with 100 ng of each compound ((B) green color).
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