摘要
目的 建立了超高效液相色谱-三重四级杆串联质谱法测定土豆以及薯片中α-茄碱与α-卡茄碱含量的方法。方法 样品经5%乙酸溶液提取,Waters Oasis C18 SPE柱(600cc)净化后,采用Waters BEH HILIC 色谱柱(100mm×2.1mm,1.7μm)分离。流动相为乙腈∶水(含10mmol/L乙酸铵)=88∶12(V/V),流速0.3ml/min。以waters Xevo TQ-S三重四级杆质谱仪在电喷雾正离子化(ESI+)及MRM模式下定量。结果 α-茄碱在0.5~500ng/ml范围内呈线性相关。方法精密度良好(RSD〈10%,n=6),回收率〉80%,α-茄碱和α-卡茄碱定量限分别为0.7和0.35μg/kg(S/N=10)。结论 本方法快速简单,重现性好,灵敏度高,适合于土豆和薯片中α-茄碱和α-卡茄碱的检测。
Objective An ultra high performance liquid chromatography-tandem quadrupole mass spectrometry (UPLC-MS/MS) method was developed for the determination of α-solanine and α-chaconine in potato tuber.MethodsThe sample was extracted with 5% acetic aicd and purified with C18 SPE column(600cc). The extraction was separated on a waters BEH HILIC column (100mm ×2.1mm,1.7μm) using 88% acetonitrile with 10mmol/L ammonium acetate as mobile phase at 0.3ml/min. The detection was performed with waters Xevo TQ-S using postive electrospray ionization (ESI+) mode and multiple-reaction monitoring (MRM) mode.ResultsThe results showed that the linear range for α-solanine was 0.5-500ng/ml. The LOQ for α-solanine was 0.7and 0.35μg/kg for α-chaconine. The method showed good accuracy with RSD〈10% (n=6) and recovery〉80%.ConclusionThis method is fast, simple and has good reproducibility. It is suitable for α-solanine and α-chaconine determination in potato tuber and crisps.
出处
《中国食品卫生杂志》
北大核心
2014年第3期233-237,共5页
Chinese Journal of Food Hygiene
基金
国家重点基础研究发展计划(973计划)(2012CB720804)