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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

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

J Mass Spectrom. 2018 Mar;53(3):240-246.

PMID: 29285822

Abstract:

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.

Chemicals Related in the Paper:

Catalog Number	Product Name	CAS Number	Price
AP1142191852	6-Bromo-2-chloro-3-(trimethylsilyl)pyridine	1142191-85-2	Price
AP1203498923	2-Chloro-5-methyl-3-(trimethylsilyl)pyridine	1203498-92-3	Price
AP25561302	N,O-Bis(trimethylsilyl)trifluoroacetamide with trimethylchlorosilane	25561-30-2	Price

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