Multi-Target Analysis and Suspect Screening of Xenobiotics in Milk by UHPLC-HRMS/MS

Abstract

The development of suspect or non-target screening methods to detect xenobiotics in biological fluids is essential to properly understand the exposome and assess its adverse health effects on humans. In order to fulfil that aim, the biomonitorization of human fluids is compulsory. However, these methods are not yet extensively developed, especially for polar organic xenobiotics in biofluids such as milk, as most works are only focused on certain analytes of interest. In this work, a multi-target analysis method to determine 245 diverse xenobiotics in milk by means of Ultra High Performance Liquid Chromatography (UHPLC)-qOrbitrap was developed. Under optimal conditions, liquid milk samples were extracted with acetonitrile in the presence of anhydrous Na2SO4 and NaCl, and the extracts were cleaned-up by protein precipitation at low temperature and Captiva Non-Drip (ND)—Lipids filters. The optimized method was validated at two concentration-levels (10 ng/g and 40 ng/g) obtaining satisfactory figures of merit for more than 200 compounds. The validated multi-target method was applied to several milk samples, including commercial and breast milk, provided by 4 healthy volunteers. Moreover, the method was extended to perform suspect analysis of more than 17,000 xenobiotics. All in all, several diverse xenobiotics were detected, highlighting food additives (benzothiazole) or phytoestrogens (genistein and genistin) in commercial milk samples, and stimulants (caffeine), plasticizers (phthalates), UV filters (benzophenone), or pharmaceuticals (orlistat) in breast milk samples.

Comparative study of characteristic compounds of three species of truffle

“…As shown in Table S1, UHPLC-Q/Orbitrap HRMS analysis based on databases (mzCloud, mzVault) and reference literature identified 87 compounds from the extract of truffles, among which 67 were identified in positive ion mode and 20 were identified in negative ion mode. The identified components contained 16 amino acids, 26 organic acids, 18 nucleosides, four amides, eight alkaloids, and 15 other types of compounds [13,15,[17][18][19][20][21][22][23][24][25][26][27][28][29][30][31][32][33][34][35]. (The total ion chromatograms, acquired within both the positive and negative ionization modes from truffle sample extracts, are displayed in Figure 1).…”

From target analysis to suspect and non-target screening of endocrine-disrupting compounds in human urine

“…The only difference was the absence of the column used for filtering the mobile phase due to steric inconveniences in the loop. Regarding qOrbitrap operating conditions, they were set according to the experience of the research group without further optimisation [43] and are detailed in Sect. 2.3.1 in SI.…”

“…In summary, in the case of pure standards, only 9.6% of the compounds (8 out of 83) could be considered false negatives using the established criteria, while 12.5% of the analytes included in the target method were not screened (3 out of 24). As for the calculation of iLOIs in human matrices, it is worth mentioning that there is a huge gap in the literature in that area [43], since LOIs have been mainly calculated in environmental matrices. The absence of LOIs in human matrices confirms the lack of harmonization in QC/QA measurements in STNS, as it has been previously stated by other experts in the field [39].…”

Applications of Chromatographic Techniques in Food and Environmental Analysis

“…The potential of the combination of target and untargeted analysis using UHPLC-MS with a Q-orbitrap as the analyzer was described and demonstrated by Musatadi et al [9] for the analysis of xenobiotics in very complex matrices, such as commercial and breast milk.…”