CAJ | 학술논문

建立了超高效液相色谱-线性离子阱／静电场轨道阱高分辨质谱检测葡萄酒中38种多酚化合物的检测方法。样品过聚醚砜（ PES）滤膜后直接上样分析，Hypersil Gold C18色谱柱分离，以乙腈（含0.1％甲酸）和0.1％甲酸水作为流动相梯度洗脱。在 m／z 50~1000范围内进行一级质谱全扫描。以准分子离子峰的精确质量数和提取的色谱图峰面积进行筛查分析和定量，以保留时间和数据依赖扫描（ data-dependent scan）模式获得的子离子质谱图进行定性确证。38种多酚化合物的质量偏差不大于5×10-6（5 ppm），浓度与特征离子峰面积的线性关系良好（浓度线性范围为两个数量级），相关系数（R2）大于0.99，方法检出限为0.002~0.50 mg／kg。3个添加水平的回收率范围为90％~102％，相对标准偏差为0.51％~2.56％。应用该方法检测了葡萄酒中38种多酚化合物的含量，该方法准确、可靠。
건립료초고효액상색보-선성리자정／정전장궤도정고분변질보검측포도주중38충다분화합물적검측방법。양품과취미풍（ PES）려막후직접상양분석，Hypersil Gold C18색보주분리，이을정（함0.1％갑산）화0.1％갑산수작위류동상제도세탈。재 m／z 50~1000범위내진행일급질보전소묘。이준분자리자봉적정학질량수화제취적색보도봉면적진행사사분석화정량，이보류시간화수거의뢰소묘（ data-dependent scan）모식획득적자리자질보도진행정성학증。38충다분화합물적질량편차불대우5×10-6（5 ppm），농도여특정리자봉면적적선성관계량호（농도선성범위위량개수량급），상관계수（R2）대우0.99，방법검출한위0.002~0.50 mg／kg。3개첨가수평적회수솔범위위90％~102％，상대표준편차위0.51％~2.56％。응용해방법검측료포도주중38충다분화합물적함량，해방법준학、가고。
Wine has been described previously as a rich source of polyphenols. However,an accurate screening of its complete phenolic profile is still lacking. In the present work,the anal-ysis of 38 polyphenols in wine using ultra high performance liquid chromatography-linear ion trap/orbitrap high resolution mass spectrometry ( UPLC-LTQ/Orbitrap MS ) was explored. Wines were directly detected. The sample was loaded onto a Thermo Hypersil Gold C18 column (100 mm × 2. 1 mm,1. 9 μm)using a gradient elution of acetonitrile/water containing 0. 1%( v/v)formic acid for the separation. UPLC-LTQ/Orbitrap mass spectrometer acquired full scan MS date for quantification,and data dependent MS2 product ion spectra for identification and/or confirmation. The regression coefficients(R2)for the calibration curves(two orders of mag-nitude up to the lowest calibration level)in the study were ≥0. 99. The limits of detection for the 38 compounds were 0. 002-0. 50 mg/kg. The average recoveries at three spiked levels were in the range of 90%-102% with the relative standard deviations( RSDs)of 0. 51%-2. 56%. Mass errors were always ≤ 5 ppm. This procedure was then successfully applied to the analysis of the polyphenols in wines.