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Volume 8, Issue 5 (Suppl)

J Chromatogr Sep Tech, an open access journal

ISSN: 2157-7064

Chromatography 2017

August 07-09, 2017

August 07-09, 2017 | Rome, Italy

4

th

World Congress on

Chromatography

Development of LC-Q-TOF-MS and LC-MS/MS method for the determination of grayanotoxins in

foodstuffs and its application to food science study

Taeik Hwang, Dongwoo Shin, Eunyoung Noh, Ji Hye Jeong, Jun Hyoung Kim, Hyoung Joon Park, Seok Heo, Jeonghwa Jo, Nam Sook Kim, Ji Hyun Lee,

Sung Kwan Park, Seong soo Park

and

Sun Young Baek

Ministry of Food and Drug Safety, Republic of Korea

A

sensitive and specific high-performance liquid chromatography–Quadrupole-time of flight mass spectrometry (LC-

Q-TOF-MS) and liquid chromatography–tandem mass spectrometry (LC-MS/MS) method was developed for the

determination of grayanotoxin I (GTX I) and grayanotoxin III (GTX III) in foodstuffs. Grayanotoxins (GTXs) were extracted

from foodstuffs via solid-phase extraction using HLB solid-phase extraction cartridges. LC-Q-TOF-MS was used to determine

the fragmentation patterns of GTXs and to characterize their fragmentation pathways. LC-MS/MS method was developed and

validated for quantitative determination of GTX I and GTX III in foodstuffs. Separation of LC-Q-TOF-MS was made using

a Waters ACQUITY BEH C18 column (100 × 2.1 mm, 1.7 μm) and separation of LC-MS/MS was made using a Capcell pack

MG II C18 column (2.0 mm × 100 mm, 3 μm). The mobile phase consisted of distilled water (v/v, A) and methanol (v/v, B)

containing 0.1% formic acid. Electrospray ionization mass spectrometry was operated in the positive ion mode. The calibration

curves of LC-MS/MS obtained were linear over the concentration range of 10–100 ng/mL (GTX I), 20-400 ng/mL (GTX III)

with a lower limit of quantification of 7.5 ng/mL (GTX I) and 15 ng/mL (GTX III), respectively. The relative standard deviation

of intra-day and inter-day precision was below 10.35% and accuracy ranged from 83.7 to 112.0%. The analytes were stable

in the stability studies. An investigation of 51 foodstuffs from the online and offline market reveals the presence of GTXs. A

quantitative estimation indicated total toxin concentrations of 1.84-101 ng/mL (GTX I) and 1.53-37.4 ng/mL (GTX III) in

foodstuffs. The potential of this approach is especially demonstrated by the fact that at least two of these toxins have not been

previously described in the literature. The validated method was successfully applied to the quantification study of GTXs in

foodstuffs for the first time.

Biography

Taeik Hwang is working as Scientific Officer at Food and Drug Safety evaluation in Ministry of Food and Drug Safety. He completed his Masters from Soonchunhyang

University in Korea.

taelee93@korea.kr

Taeik Hwang et al., J Chromatogr Sep Tech 2017, 8:5(Suppl)

DOI: 10.4172/2157-7064-C1-032