IU CINQUIMA, Analytical Chemistry Group, University of Valladolid, 47011 Valladolid, Spain.
IU CINQUIMA, Analytical Chemistry Group, University of Valladolid, 47011 Valladolid, Spain.
Food Chem. 2014;152:66-74. doi: 10.1016/j.foodchem.2013.11.125. Epub 2013 Nov 28.
A new method has been developed and validated to determine twelve intact glucosinolates (glucoiberin, GIB; glucoraphanin, GRA; glucoerucin GER; gluconapin, GNA; glucotropaeolin, GTL; glucobrassicin, GBC; gluconasturtiin, GST; glucoalyssin, ALY; 4-hydroxyglucobrassicin, 4-OH; 4-metoxyglucobrassicin, 4ME; neoglucobrassicin, NEO; sinigrin, SIN) in broccoli leaves using liquid chromatography (LC) coupled to diode array (DAD) and electrospray ionization mass spectrometry (ESI-MS) detection. An extraction procedure has also been proposed and optimized by means of statistical analysis (the Box-Behnken design and analysis of variance); this is based on the deactivation of myrosinase using a microwave and heated water. Low limits of detection and quantification were obtained, ranging from 10 to 72 μg/g with DAD and 0.01 to 0.23 μg/g with ESI-MS, and the resulting recovery values ranged from 87% to 106% in all cases. Finally, glucosinolates were analyzed in broccoli leaf samples from six different cultivars (Ramoso calabrese Parthenon, Marathon, Nubia, Naxos and Viola).
已开发并验证了一种新方法，用于测定十二种完整的硫代葡萄糖苷（葡萄糖苷，GIB；萝卜硫素，GRA；葡萄糖异硫氰酸酯，GER；葡萄糖苷，GNA；葡萄糖芸苔素，GTL；硫代葡萄糖苷，GBC；葡萄糖芥子油苷，GST；丙硫氨酸芥子油苷，ALY；4-羟基硫代葡萄糖苷，4-OH；4-甲氧基硫代葡萄糖苷，4ME；新葡萄糖苷，NEO；黑芥子硫苷酸钾，SIN）在西兰花叶中的含量，采用液相色谱（LC）与二极管阵列（DAD）和电喷雾电离质谱（ESI-MS）检测相结合的方法。还通过统计分析（Box-Behnken 设计和方差分析）提出并优化了一种提取程序；该程序基于使用微波和热水使黑芥子酶失活。使用 DAD 可获得 10 至 72 μg/g 的低检测限和定量限，使用 ESI-MS 可获得 0.01 至 0.23 μg/g 的低检测限和定量限，所有情况下的回收率值均在 87%至 106%之间。最后，对来自六个不同品种（Ramoso calabrese Parthenon、Marathon、Nubia、Naxos 和 Viola）的西兰花叶样品中的硫代葡萄糖苷进行了分析。
