高效液相色谱-串联质谱法测定茄科蔬菜及其制品中α-茄碱和α-卡茄碱的含量

Determination of α-solanine and α-chaconine in solanaceous vegetables and their products by high performance liquid chromatography-tandem mass spectrometry

中文关键词:  α-茄碱  α-卡茄碱  通过式固相萃取  高效液相色谱-串联质谱法  茄科蔬菜

英文关键词:α-solanine  α-chaconine  pass-through solid phase extraction  high performance liquid chromatography-tandem mass spectrometry  solanaceous vegetables

中文摘要:

      目的 建立通过式固相萃取-高效液相色谱-串联质谱法同时测定茄科蔬菜及其制品中α-茄碱和α-卡茄碱含量的分析方法。方法 样品采用1%甲酸水溶液:乙腈=1:1 (V:V)涡旋提取, Oasis? PRiME HLB固相萃取(solid phase extraction, SPE)柱净化, 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(A): 2 mmol/L乙酸铵的乙腈溶液(B)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, 基质匹配标准曲线外标法定量。结果 在1~500 ng/mL范围内, α-茄碱和α-卡茄碱与峰面积线性关系良好(相关系数r2>0.998)。在低、中、高3个水平添加下, α-茄碱回收率为91.3%~104.6%, α-卡茄碱回收率为90.3%~108.4%, 相对标准偏差不超过5.5% (n=6)。结论 该方法快速简便、准确度好、灵敏度高, 适用于大批量茄科蔬菜及其制品中α-茄碱和α-卡茄碱的快速测定。

英文摘要:

      Objective To establish a method for the the simultaneous determination of α-solanine and α-chaconine in solanaceous vegetables and products of solanaceous vegetable by pass-through solid phase extraction-high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Methods The sample was extracted with 1% formic acid solution : acetonitrile 1:1 (V:V) and purified by Oasis? PRiME HLB SPE column, which was separated by BEH Amide chromatographic 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 (A) and 2 mmol/L ammonium formic acid solution acetonitrile solution (B) 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 quantified by matrix-matched external standard curves. Results α-solanine and α-chaconine had good linear relationships with peak area in the concentration of 1?500 ng/mL (r2>0.998). The average recoveries of α-solanine and α-chaconine were 91.3%?104.6% and 90.3%?108.4% at the low, middle and high spiked levels, and the relative standard deviations were no more than 5.5% (n=6). Conclusion This method is rapid and simple, accurate and sensitive, which is suitable for rapid determination of α-solanine and α-chaconine in a large scale solanaceous vegetables and products of solanaceous vegetable