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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
Author(s) -
Nagy Tibor,
Kuki Ákos,
Nagy Lajos,
Zsuga Miklós,
Kéki Sándor
Publication year - 2018
Publication title -
journal of mass spectrometry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.475
H-Index - 121
eISSN - 1096-9888
pISSN - 1076-5174
DOI - 10.1002/jms.4061
Subject(s) - chemistry , silylation , derivatization , bstfa , rutin , pyridine , chromatography , dart ion source , trimethylsilyl , mass spectrometry , acetamide , organic chemistry , electron ionization , catalysis , ion , ionization , antioxidant
Direct analysis in real‐time mass spectrometry (DART‐MS) with in situ silylation was used for the rapid analysis of the flavonoids silybin ((2 R ,3 R )‐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.