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目的建立超高效液相色谱串联质谱法检测土豆及其制品中α-茄碱的分析方法。方法通过优化提取液,土豆样品经1%甲酸-甲醇(1:1,V:V)超声提取,采用BEH C_(18)色谱柱(2.1 mm×50 mm,1.7μm)分离,梯度洗脱,采用超高效液相色谱串联质谱法,在多反应监测模式进行定性和定量分析,而土豆淀粉用MCX固相萃取柱进行净化,液相色谱串联质谱法测定。结果土豆样品中回收率为75%~115%,相对标准偏差为5.0%~8.6%,土豆淀粉的回收率范围为67%~100%,相对标准偏差为3.4%~11.3%,方法的检出限和定量限分别为0.5 mg/kg和1.0 mg/kg。结论该方法适合于土豆及其制品中α-茄碱的分析。
OBJECTIVE To establish a method for the determination of α-solanine in potatoes and their products by ultra performance liquid chromatography-tandem mass spectrometry. Methods The samples were extracted with 1% formic acid - methanol (1: 1, V: V) and analyzed by BEH C 18 column (2.1 mm × 50 mm, 1.7 μm) Qualitative and quantitative analysis was performed in a multi-reaction monitoring mode using ultra performance liquid chromatography-tandem mass spectrometry, while potato starch was purified using a MCX solid phase extraction column and determined by liquid chromatography tandem mass spectrometry. Results The recoveries of potato samples ranged from 75% to 115% with relative standard deviations from 5.0% to 8.6%. The recovery rates of potato starch ranged from 67% to 100% and the relative standard deviations ranged from 3.4% to 11.3% Limit and limit of quantification were 0.5 mg / kg and 1.0 mg / kg, respectively. Conclusion The method is suitable for the analysis of α-solanine in potatoes and their products.