摘要
【目的】建立常见十字花科蔬菜中抗癌活性物吲哚-3-甲醇(I3C)的液相色谱-串联质谱(LC-MS/MS)检测方法。【方法】样品经均质、磷酸缓冲罐溶液孵育水解,取1 mL水解液,用3 mL乙酸乙酯分3次萃涡旋萃取,氮气吹干,甲醇复溶,LC-MS/MS多反应监测(MRM)模式检测,外标法定量。【结果】检测方法线性良好,R^(2)>0.999,检出限(LOD)为0.040μg/g,定量限为0.133μg/kg,加标回收率为88.12%~109.8%,相对标准偏差为1.96%~7.78%;对6种不同产地的十字花科蔬菜的实际检测显示,I3C平均含量在1.5μg/g以上的有在西兰花和羽衣甘蓝,平均含量为0.5~1.5μg/g的有圆白菜、菜花和紫甘蓝,低于0.5μg/g的为油菜。【结论】该方法有效简化了样品前处理,提高了检测效率,有更低的检出限和定量限,为相关蔬菜I3C含量检测提供了方法参考;实际样品的检测结果,为健康饮食或调理食材的选择提供了依据。
[Objective]To establish a liquid chromatography-tandem mass spectrometry(LC-MS/MS)method for the determination of indole-3-carbinol(I3C),an anticancer active compound in common cruciferous vegetable.[Method]With homogenizing,incubating and hydrolyzing with phosphoric acid buffer solution,I3C was extracted 3 times from 1 mL of the hydrolysate by 1ml of ethyl acetate each time.Then the extract was dried with nitrogen blowing and reconstituted with methanol,and I3C was determined by liquid chromatography-tandem mass spectrometry(LC-MS/MS)in multiple reaction monitoring(MRM)mode.The quantification was carried with external standard method.[Results]The method established was linearity with R^(2)>0.999;The limit of detection(LOD)is 0.040μg/g;the limit of quantification(LOQ)is 0.133μg/g;the recoveries were 88.12%-109.8%with the relative standard deviation rang of 1.96%-7.78%.The actual tests of 6 cruciferous vegetables with different origins showed that the average content of I3C was more than 1.5μg/g in broccoli and kale,the average content was 0.5-1.5μg/g in cabbage,cauliflower and purple cabbage,and the average content was less than 0.5μg/g in oilseed rape.[Conclusion]This method effectively simplified the sample preparation,improved the detection efficiency,and had lower detection and quantification limits,which provided a method reference for the detection of I3C content in related vegetables.The actual sample test results provides a basis for the selection of healthy diet or conditioning ingredients.
作者
赵毅
王宗义
赵青原
张巍青
马小童
董子琦
吴建欣
ZHAO Yi;WANG Zongyi;ZHAO Qingyuan;ZHANG Weiqing;MA Xiaotong;DONG Ziqi;WU Jianxin(Beijing Key Laboratory of Agricultural Product Detection and Control for Spoilage Organisms and Pesticides,College of Food Sciences and Engineering,Beijing University of Agriculture,Beijing,102206,China;Guangzhou Hexin Instrument Co.,Ltd,Guangzhou 510535,China;China National Research Institute of Food&Fermentation Industries Co.Ltd.Beijing 100015,China)
出处
《北京农学院学报》
2025年第2期102-105,共4页
Journal of Beijing University of Agriculture
基金
北京市都市农林学交叉学科平台建设项目
北京农学院教改重点项目“服务乡村振兴专业能力实训课程体系的构建与教学实践”(5046516654/149)。
关键词
吲哚-3-甲醇
十字花科蔬菜
液相色谱-串联质谱法
indole-3-carbinol
cruciferous vegetables
liquid chromatography-tandem mass spectrometry
