科研之友
微信
新浪微博
Facebook
分享链接
摘要
Objectives: Although general unknown screening (GUS) is often used to detect and identify exogenous compounds in biological matrices, some compounds are not detected for two main reasons: first the method carried out for the extraction, secondly, the lack of sensitivity in the detection of the unknown molecules. The aim of this study was to improve the detection, using an acidic extraction procedure and a MRM mode (ES+ or ES ). Methods: Blank sera were spiked with 42 substances, not detected in GUS. 1 mL was extracted after addition of internal standards and 500 米L of acetate buffer by 3 mL of organic extraction solution (dichloromethane: ether: hexane: isoamyl alcohol; 30:50:20:0.5, v/v). Basic extraction was also carried out by substituting the sodium acetate buffer with saturated borate buffer. The extracts were analysed by UPLC-MS-MS, using MRM mode (ES+ or ES ). Results: All the non detected substances by the GUS method were indentified in this study, 25 in ES+ mode and 17 in ES mode. Extraction yield was between 9 and 104%, and upper, compared to that after basic extraction. Conclusion: A rapid, sensitive and selective method using positive or negative MRM mode, with a triple quadrupole mass spectrometer and a simple acidic liquid-liquid extraction allows to identify, confirm and quantify 42 substances (drugs and pesticides) not detected by a routine GUS method. Objectifs: Bien que le screening large soit souvent utilis谷 pour d谷tecter et identifier les compos谷s exog豕nes dans les matrices biologiques, certains compos谷s ne sont pas d谷tect谷s pour deux raisons principales : une m谷thode d＊extraction utilis谷e non adapt谷e et un manque de sensibilit谷 dans la d谷tection pour les compos谷s inconnus. Le but de cette 谷tude a 谷t谷 d＊am谷liorer la d谷tection en utilisant une m谷thode d＊extraction acide et le mode MRM (ES+ ou ES ). M谷thodes : Le blanc s谷rum a 谷t谷 surcharg谷 avec 42 substances, non d谷tect谷es par le screening de recherche large. 1 mL d＊谷chantillon en pr谷sence d＊谷talons internes a 谷t谷 extrait avec 500 米L de tampon ac谷tate et 3 mL d＊un m谷lange de solvants (dichlorom谷thane/ether/hexane/alcool isoamylique 30/50/20/0,5 v/v). L＊extraction basique a 谷galement 谷t谷 谷valu谷e en substituant le tampon ac谷tate par du tampon borate. Les extraits sont analys谷s par UPLC-MS/MS, en utilisant le mode MRM (ES+ ou ES ). R谷sultats : Tous les compos谷s non d谷tect谷s par la m谷thode screening large ont 谷t谷 identifi谷s dans cette 谷tude, 25 en mode ES+ et 17 en mode ES . Les rendements d＊extraction 谷taient compris entre 9 et 104 %, et sup谷rieurs 角 ceux obtenus apr豕s extraction basiqu
