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

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BEHAmide (2.1mm×100 mm, 1.7μm)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0.4m L/min,多反应模式监测,外标法定量。结果α-茄碱和α-卡茄碱在5~1000ng/m L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。

Objective To establish a method for determination of solanineα-solanine andα-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:acetonitrile1:1(V:V)and purified by matrix solid-phase dispers of C18,which was separated by BEH amidechromatographic column(2.1 mm×100 mm,1.7μm),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 m L/min.It was monitored by multi reaction mode,and quantitatively analyzed by external standard method.Results Theα-solanine andα-chaconine had good linear relationships in the concentration of 5-1000 ng/m LThe limits of detection and limits of quantitation ofα-solanin were 0.1-1 mg/kg and 0.3-3 mg/kg,respectively.The limits of detection and limits of quantitation ofα-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 ofα-solanine were 90.7%-108.0%,the recoveries ofα-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 ofα-solanine andα-chaconine in a large scale solanaceous vegetables and products of solanaceous vegetable.