高效液相色谱-串联质谱法检测新鲜芝麻菜中芝麻菜苷

Determination of glucoerucin in fresh Eruca sativa Mill by high performance liquid chromatography-tandem mass spectrometry

中文关键词:  芝麻菜苷  芝麻菜  高效液相色谱-串联质谱法

英文关键词:glucoerucin  Eruca sativa Mill  high-performance liquid chromatography-tandem mass spectrometry

中文摘要:

      目的 建立高效液相色谱-串联质谱法(high-performance liquid chromatography-tandem mass spectrometry, HPLC-MS/MS)测定新鲜芝麻菜中芝麻菜苷的检测新技术。方法 芝麻菜样品采用80% (V:V)甲醇-水在70 ℃水浴下振荡提取20 min, 离心取上清液于45 ℃氮气条件下吹干, 超纯水超声复溶, 以0.1%甲酸水溶液-乙腈为流动相进行梯度洗脱, 经C18色谱柱进行分离, 采用电喷雾负离子多反应监测模式(multiple response monitoring, MRM)对新鲜芝麻菜中芝麻菜苷进行检测, 外标法定量。结果 芝麻菜苷在10~500 ng/mL浓度范围内线性良好(r2≥0.998), 检出限为3.0 μg/kg, 定量限为10.0 μg/kg, 新鲜芝麻菜中加标回收率为92.1%~101.0%, 相对标准偏差为3.86%。应用本研究建立的方法对不同生长周期芝麻菜中芝麻菜苷含量检测, 其含量及变化趋势与文献报道基本一致。结论 本方法操作简便、灵敏度和回收率高、重复性好, 适用于新鲜芝麻菜中芝麻菜苷的检测。

英文摘要:

      Objective To establish a method for the determination of glucoerucin in Eruca sativa Mill by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Methods The samples were extracted with 80% (V:V) methanol-water in 70 ℃ water bath for 20 min. After centrifugation, the supernatant was dried in nitrogen at 45 ℃ and ultrasonically dissolved in ultrapure water, and separated on a C18 column using 0.1% formic acid aqueous solution and acetonitrile as mobile phase, glucoerucin in fresh Eruca sativa was detected by electrospray negative ion and multiple response monitoring (MRM) mode, and quantified by external standard method. Results The linear range of glucoerucin was 10?500 ng/mL (r2≥0.998). The limit of detection was 3.0 μg/kg, and the limit of quantification was 10.0 μg/kg. The recoveries of fresh Eruca sativa Mill were 92.1%?101.0%, and the relative standard deviation was 3.86%. The method established in this study was applied to determine the content of glucoerucin in Eruca sativa Mill of different growth cycles, and content and changing trend were basically consistent with the literature reports. Conclusion This method is sample, sensitive and repeatable, and can be used for the determination of glucoerucin in Eruca sativa Mill.