TY - JOUR
T1 - μSPE followed by HPLC–MS/MS for the determination of series D and E resolvins in biological matrices
AU - Fanti, Federico
AU - Oliva, Eleonora
AU - Tortolani, Daniel
AU - Di Meo, Camilla
AU - Fava, Marina
AU - Leuti, Alessandro
AU - Rapino, Cinzia
AU - Sergi, Manuel
AU - Maccarrone, Mauro
AU - Compagnone, Dario
N1 - Funding Information:
Italian Ministry of Health (Grant Ricerca Finalizzata 2018 - n. RF-2018-12365391) to Mauro Maccarrone.
Publisher Copyright:
© 2021 Elsevier B.V.
PY - 2021/9/5
Y1 - 2021/9/5
N2 - The critical role of acute inflammatory processes is recognized in many chronic diseases; a key point in molecular mechanisms of acute inflammation resolution is represented by a new group of pro-resolving lipid mediators that include distinct families of molecules: lipoxins, resolvins, protectins and maresins, collectively termed “specialized pro-resolving mediators” (SPMs). In particular, resolvins are active in the picogram to nanogram dose range, whereby they can directly modulate a plethora of anti-inflammatory responses. The presented method proposes an analytical protocol able to extract and to quantify 6 different resolvins from 3 different matrices (plasma, cells and exudates). The method, validated according to the EMA guideline for bioanalysis, exhibited good precision (1%–20%) and accuracy (2%–20%). In particular, the combination of two different sample preparation techniques, Liquid-Liquid Extraction (LLE) and micro-Solid Phase Extraction (μSPE), applied for the first on this class of molecules, used for the extraction and clean-up respectively, led to high enrichment factor (20 fold) and consequently a high sensitivity (LOQ between 1 and 38 pg mL−1); moreover the validation data proved the versatility of μSPE as clean-up tool as it was capable to manage huge enrichment factor without negatively affect accuracy and precision of analysis.
AB - The critical role of acute inflammatory processes is recognized in many chronic diseases; a key point in molecular mechanisms of acute inflammation resolution is represented by a new group of pro-resolving lipid mediators that include distinct families of molecules: lipoxins, resolvins, protectins and maresins, collectively termed “specialized pro-resolving mediators” (SPMs). In particular, resolvins are active in the picogram to nanogram dose range, whereby they can directly modulate a plethora of anti-inflammatory responses. The presented method proposes an analytical protocol able to extract and to quantify 6 different resolvins from 3 different matrices (plasma, cells and exudates). The method, validated according to the EMA guideline for bioanalysis, exhibited good precision (1%–20%) and accuracy (2%–20%). In particular, the combination of two different sample preparation techniques, Liquid-Liquid Extraction (LLE) and micro-Solid Phase Extraction (μSPE), applied for the first on this class of molecules, used for the extraction and clean-up respectively, led to high enrichment factor (20 fold) and consequently a high sensitivity (LOQ between 1 and 38 pg mL−1); moreover the validation data proved the versatility of μSPE as clean-up tool as it was capable to manage huge enrichment factor without negatively affect accuracy and precision of analysis.
KW - Biological matrices
KW - HPLC–MS/MS
KW - Liquid-liquid extraction
KW - Micro-SPE
KW - Resolvins
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U2 - 10.1016/j.jpba.2021.114181
DO - 10.1016/j.jpba.2021.114181
M3 - Article
AN - SCOPUS:85107425295
VL - 203
JO - Journal of Pharmaceutical and Biomedical Analysis
JF - Journal of Pharmaceutical and Biomedical Analysis
SN - 0731-7085
M1 - 114181
ER -