The chemical informs about 70 individual phenolic compounds were constructed from various lettuce samples based on literature sources and analytical data. A total of 30 phenolic compounds including quercetin 3-O-glucuronide, quercetin 3-O-(6''-O- malonyl) glucoside, cyanidin 3-O-(6''-O-malonyl)glucoside, chlorogenic acid and chicoric acid as major components were identified in 6 lettuce samples from Korea using UPLC-DAD-QToF/MS on the basis of constructed library. Among these, quercetin 3,7-di-O-glucoside(m/z 627 [M+H]+), quercetin 3-O-(2''-O-malonyl)glucoside(morkotin C, m/z 551 [M+H]+), quercetin 3-O-(6''- O-malonyl)glucoside methyl ester(m/z 565 [M+H]+), 5-O-cis-p-coumaroylquinic acid(m/z 339 [M+H]+) and 5-O-caffeoylquinic acid methyl ester(m/z 369 [M+H]+) were newly confirmed from the lettuce samples. In total content of phenolic compounds, 4 red lettuce samples(2,947.7~7,535.6 mg/100 g, dry weight) showed higher than green lettuce(2,687.3 mg) and head lettuce(320.1 mg).
본 연구는 건강기능식품 프랑스해안송껍질추출물 중 catechin, caffeic acid, ferulic acid, taxifolin에 대한 동시분석법을 개발하는 연구이다. 최적분석조건을 확립하기 위해 시료 채취량, 용매 조건을 비교 검토하였으며, UPLCMS/ MS를 이용하여 각 4개 성분에 대한 정확한 분석 및 분석시간의 효율성도 향상하였다. 분석 시 사용한 컬럼은 Acquity UPLC BEH C18이며, 정량이온으로 catechin, caffeic acid, ferulic acid, taxifolin 각각 133, 135, 245 및 248을 선정하였다. 확립된 시험법에 대해 특이성, 직선성, 검출한계, 정량한계, 정확성, 정밀성 등의 밸리데이션을 수행하였다. 4개 성분 모두 50-25000 mg/L 농도에서 결정계수(R2) 0.999이상으로 높은 직선성을 확인하였다. 또한 회수율은 84.9-104%이었고, 정밀성은 1.2-4.3%의 RSD를 확인하였다. 개발된 시험법은 프랑스해안송껍질추출물 중 catechin, caffeic acid, ferulic acid, taxifolin 분석을 위한 시험법으로 활용되기에 적합한 것으로 판단된다.
Background : The 1,2-unsaturated PAs, reported to be widely present in medicinal plants belonging to Asteraceae, Boraginaceae, and Fabaceae, cause hepatotoxicity and genotoxicity in humans and animals. Hence, there is a need for an analytical method that allows these dangerous plant toxins to be determined. In this study, we developed a method that can be used for the rapid and accurate determination of nine toxic PAs in medicinal plants using ultra-pressure liquid chromatography–electrospray ionization–quadrupole–time-of-flight mass spectrometry (UPLC-ESI-Q-TOF).
Methods and Results : The compounds were eluted onto a C18 column with 0.1% formic acid and acetonitrile, and separated with good resolution within 11 min. all analytes was characterized by its precursor ions generated by ESI-Q-TOF and fragment ions produced by collision-induced dissociation (CID), which were used as a reliable database. The proposed analytical method was verified with reference to the ICH guidelines. The proposed UPLC-ESI-Q-TOF method was applied to four medicinal plants, and lycopsamin, echimidine, senkirkine and senecionine were detected by matching with reference standard, and additional six PAs were tentatively identified though chemical profiling. In addition, the QuEchERS method was the most efficient in comparison with methods like hot water and methanol in extraction efficiency of pyrrolizidine alkaloids.
Conclusion : The our proposed method can determine PAs rapidly and accurately in medicinal plants and will be utilize as an important data for other researchers who need analytical information of PAs.