基于固相基质分散的高效液相色谱-串联质谱法测定茄科蔬菜及其制品中龙葵素的含量

Determination of solanine in solanaceous vegetables and products of solanaceous vegetable by high performance liquid chromatography-tandem mass spectrometry based on solid phase matrix dispersion

中文关键词:  茄科蔬菜  龙葵素  固相基质分散  高效液相色谱-串联质谱法

英文关键词:solanaceous vegetables  solanine  matrix solid-phase disperse  high performance liquid chromatography- tandem mass spectrometry

中文摘要:

      目的 建立高效液相色谱-串联质谱法测定茄科蔬菜及其制品中龙葵素α-茄碱和α-卡茄碱含量。 方法 样品采用0.1%甲酸水溶液:乙腈=1:1(V:V)提取, C18固相基质分散净化, 经过色谱柱BEH Amide (2.1 mm ×100 mm, 1.7 μm)分离, 以2 mmol/L乙酸铵的0.1%甲酸水溶液: 2 mmol/L乙酸铵的乙腈溶液为流动相进行梯度洗脱, 柱温40 ℃, 流速0.4 mL/min, 多反应模式监测, 外标法定量。结果 α-茄碱和α-卡茄碱在5~1000 ng/mL内线性关系良好(r2>0.999)。α-茄碱方法检出限和定量限范围分别为0.1~1 mg/kg, 0.3~3 mg/kg; α-卡茄碱检出限和定量限分别为0.03~0.3 mg/kg, 0.1~1 mg/kg; 在低、中、高3水平添加下, α-茄碱回收率为90.7%~108.0%, α-卡茄碱回收率为89.8%~102.7%, 相对标准偏差均小于5.6%(n=6)。结论 本方法快速简便、准确度好、灵敏度高等特点, 适用于大批量茄科蔬菜及其制品中α-茄碱和α-卡茄碱的测定。

英文摘要:

      Objective To establish a method for determination of solanine α-solanine and α-chaconine in solanaceous vegetables and products of solanaceous vegetable by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Methods The sample was extracted with 0.1% formic acid solution:acetonitrile 1:1(V:V) and purified by matrix solid-phase dispers of C18, which was separated by BEH amidechromatographic column (2.1 mm×100 mm, 1.7 μm), and analyzed by HPLC-MS/MS with 2 mmol/L ammonium 0.1% formic acid solution and 2 mmol/L ammonium formic acid solution acetonitrile solution as the mobile phase on gradient elution program, the column temperature was 40 ℃ and the flow rate was 0.4 mL/min. It was monitored by multi reaction mode, and quantitatively analyzed by external standard method. Results The α-solanine and α-chaconine had good linear relationships in the concentration of 5?1000 ng/mL (r2>0.999). The limits of detection and limits of quantitation of α-solanin were 0.1?1 mg/kg and 0.3?3 mg/kg, respectively. The limits of detection and limits of quantitation of α-chaconine were 0.03?0.3 mg/kg, 0.1?1 mg/kg, respectively. Under the addition of low, medium and high levels, the recoveries of α-solanine were 90.7%?108.0%, the recoveries of α-chaconine were 89.8%?102.7%, and the relative standard deviations were less than 5.6% (n=6). Conclusion This method is rapid and simple, accurate and sensitive, which is suitable for determination of α-solanine and α-chaconine in a large scale solanaceous vegetables and products of solanaceous vegetable.