Lin Yi-Reng, Huang Mei-Fang, Wu You-Ying, Liu Meng-Chieh, Huang Jing-Heng, Chen Ziyu, Shiue Yow-Ling, Wu Chia-En, Liang Shih-Shin
Department of Biotechnology, School of Environment and Life Sciences, Fooyin University, Kaohsiung, Taiwan.
Department of Biotechnology, College of Life Science, Kaohsiung Medical University, Kaohsiung, Taiwan.
Food Chem. 2017 Sep 1;230:1-5. doi: 10.1016/j.foodchem.2017.02.119. Epub 2017 Feb 27.
In this work, we synthesized internal standards for four garlic organosulfur compounds (OSCs) by reductive amination with C, D-formaldehyde, and developed an isotope dilution analysis method to quantitate these organosulfur components in garlic samples. Internal standards were synthesized for internal absolute quantification of S-allylcysteine (SAC), S-allylcysteine sulfoxide (alliin), S-methylcysteine (SMC), and S-ethylcysteine (SEC). We used a multiple reaction monitoring (MRM) to detect C, D-formaldehyde-modified OSCs by ultrahigh-performance liquid phase chromatography coupled with tandem mass spectrometry (UHPLC-MS/MS) and obtained MS spectra showing different ratios of C, D-formaldehyde-modified and H-formaldehyde-modified compounds. The resulting labeled and unlabeled OSCs were exhibited correlation coefficient (R) ranged from 0.9989 to 0.9994, respectively. The average recoveries for four OSCs at three concentration levels ranged from 89% to 105%. By C, D-formaldehyde and sodium cyanoborohydride, the reductive amination-based method can be utilized to generate novel internal standard for isotope dilution and to extend the quantitative application.
在本研究中,我们通过用C、D-甲醛进行还原胺化反应,合成了四种大蒜有机硫化合物(OSCs)的内标,并开发了一种同位素稀释分析方法来定量大蒜样品中的这些有机硫成分。为S-烯丙基半胱氨酸(SAC)、S-烯丙基半胱氨酸亚砜(蒜氨酸)、S-甲基半胱氨酸(SMC)和S-乙基半胱氨酸(SEC)的绝对定量合成了内标。我们使用多反应监测(MRM)通过超高效液相色谱-串联质谱联用(UHPLC-MS/MS)检测C、D-甲醛修饰的OSCs,并获得了显示C、D-甲醛修饰和H-甲醛修饰化合物不同比例的质谱图。所得标记和未标记的OSCs的相关系数(R)分别在0.9989至0.999之间。四种OSCs在三个浓度水平下的平均回收率在89%至105%之间。通过C、D-甲醛和氰基硼氢化钠,基于还原胺化的方法可用于生成用于同位素稀释的新型内标,并扩展定量应用。