Rapid qualitative analysis of 2 flavonoids, rutin and silybin, in medical pills by direct analysis in real-time mass spectrometry (DART-MS) combined with in situ derivatization

Tibor Nagy, Ákos Kuki, Lajos Nagy, Miklós Zsuga, Sándor Kéki

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Direct analysis in real-time mass spectrometry (DART-MS) with in situ silylation was used for the rapid analysis of the flavonoids silybin ((2R,3R)-3,5,7-trihydroxy-2-[3-(4-hydroxy-3-methoxyphenyl)-2-hydroxymethyl-2,3-dihydrobenzo[1,4]dioxin-6-yl]chroman-4-one) and rutin (quercetin-3-O-rutinoside). Three different derivatization reagents, hexamethyldisilazane/trimethylchlorosilane/pyridine (HMDS/TMCS/pyridine), N,O-bis(trimethylsilyl)acetamide/trimethylchlorosilane/N-trimethylsilyimidazole (BSA/TMCS/TMSI), and N,O-bis(trimethylsilyl)trifluoroacetamide/trimethylchlorosilane (BSTFA/TMCS), were applied. Silybin and rutin were detected with various degrees of silylation, and the formation of dimers with pyridine and imidazole was also observed. HMDS/TMCS/pyridine was the best choice for the DART-MS analysis of silybin, and BSA/TMCS/TMSI was the most effective for the detection of rutin. The effects of the DART source temperature on desorption, ionization, in-source fragmentation, dimer formation, and hydrolysis of the trimethylsilyl groups were also studied. In addition, the collision-induced dissociation properties of the derivatized silybin and rutin were explored. With our in situ silylation method, the derivatized bioactive compounds in intact medical pills could also be detected by DART-MS.

Original languageEnglish
Pages (from-to)240-246
Number of pages7
JournalJournal of Mass Spectrometry
Issue number3
Publication statusPublished - Mar 2018



  • direct analysis in real time mass spectrometry (DART-MS)
  • flavonoid derivatives
  • in situ derivatization
  • rutin
  • silybin
  • silylation

ASJC Scopus subject areas

  • Spectroscopy

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