超高效液相色谱-串联三重四极杆质谱法同时测定油菜籽中13种硫代葡萄糖苷

Simultaneous determination of 13 kinds of glucosinolates in rapeseed by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  超高效液相色谱-串联三重四极杆质谱法  硫代葡萄糖苷  油菜籽

英文关键词:ultra performance liquid chromatography-tandem mass spectrometry  glucosinolates  rapeseed

中文摘要:

      目的 建立超高效液相色谱-串联三重四极杆质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)同时测定油菜籽中13种硫代葡萄糖苷含量的分析方法。方法 菜籽样品经液氮冷冻后, 立即使用微型粉碎机进行粉碎。将粉碎好的菜籽(1 g)置入盛有甲醇-水溶液(7:3, V:V)的离心管中, 进行75 ℃水浴后, 采用超声萃取5 min。以A相为0.1%甲酸水溶液, B相为甲醇作为流动相进行梯度洗脱, 采用电喷雾离子源负离子多反应监测模式测定, 外标法定量。结果 样品中13种硫代葡萄糖苷在0.2~2.0 mg/L范围内线性关系良好, 相关系数大于0.996, 检出限为0.01~1.16 mg/kg, 定量限为0.04~3.87 mg/kg, 加标回收率为72.5%~124.0%, 相对标准偏差为2.31%~11.50%。结论 该方法操作简便, 回收率和重复性良好, 适合于油菜籽中硫代葡萄糖苷的准确定量定性分析。

英文摘要:

      Objective To establish a method for the simultaneous determination of 13 kinds of glucosinolates in rapeseed by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The rapeseed samples were chilled by liquid nitrogen and immediately crushed by a micro-pulverizer. The crushed rapeseed (1 g) placed into a centrifuge tube containing mixed solution of methanol and water (7:3, V:V), bathed at 75 ℃ for 5 min and were kept on an ultraspnic bath for extracting. The mobile phase was gradient elution with 0.1% formic acid aqueous solution (phase A) and 100% methanol (phase B). Detection was performed using an electrospray ionization source in the negative ion model with multiple reaction monitoring, and quantified by external standard method. Results The calibration curves for 13 kinds of glucosinolates were liner in the range of 0.2? 2.0 mg/L with correlation coefficients greater than 0.996. The limits of detection ranged from 0.01 to 1.16 mg/kg, the limits of quantitation ranged from 0.04 to 3.87 mg/kg, the recoveries for spiked samples were 72.5%?124.0% and the relative standard deviations ranged from 2.31% to 11.50%. Conclusion This method proves simple, fast and accurate and has relative better recoveries and repeatability. It is suitable for the fast detection of glucosinolates in rapeseed.