超高效液相色谱-三重四级杆串联质谱法测定土豆中α-茄碱与α-卡茄碱含量  

Determination of α-solanine and α-chaconine in potato by ultra high performance liquid chromatography-tandem triple quadruple mass spectrometry

作　　者：王丹 丁颢 程莉[2] 周爽 赵云峰 

机构地区：[1]国家食品安全风险评估中心,北京100021 [2]山西医科大学公共卫生学院,山西太原030001

出　　处：《中国食品卫生杂志》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)

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.

关 键 词：超高效液相色谱-串联三重四极杆质谱法 α键茄碱 α-卡茄碱 土豆 植物毒素 食品安全 

分 类 号：O657.63[理学—分析化学] TS207.3[理学—化学]