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。