同位素稀释内标GC-MS/MS法分析乳粉中三聚氰酸  

Analysis of Cyanuric Acid in Milk Powder by Gas Chromatography Tandem Triple Quadruple Mass Spectrometry with an Isotopic Internal Standard

作　　者：李东刚[1] 李春娟[1] 鞠福龙[1] 刘敬东[1] 

机构地区：[1]黑龙江省质量监督检测研究院,黑龙江哈尔滨150050

出　　处：《食品科学》2011年第10期227-231,共5页Food Science

摘　　要：建立以三聚氰酸-13C为内标,利用三重四极杆气相色谱质谱联用(GC-MS/MS)的多反应监测(MRM)技术分析乳粉中三聚氰酸的方法。三聚氰酸以甲醇提取,利用衍生化试剂BSTFA(99%)-TMCS(1%)进行衍生化处理、分析三聚氰酸衍生物的裂解规律、考察基质效应,以三聚氰酸-13C为内标、利用多反应监测(MRM)技术定量分析,三聚氰酸的定性定量离子对为m/z 345>215、345>330,对应的三聚氰酸-13C衍生物的离子对为m/z 348>217、348>333。以m/z 345>215与m/z 348>217的峰面积比值进行定量,方法在0.010～0.50mg/L范围内呈良好线性关系。三聚氰酸的检测限为0.014mg/kg,精密度为3.4%～4.8%,回收率为90.0%～102.5%,以能力验证和外标法对此方法进行考察,数据表明方法准确、可靠。The method for analyzing cyanuric acid in milk powder by gas chromatography tandem triple quadruple mass spectrometry（GC-MS/MS） with an isotopic internal standard and a multiple-reaction monitoring（MRM） system was established.The milk powder samples were extracted by methanol,and derivatized with BSTFA＋TMCS（1%）.The optimal parameters for instruments,matrix effects,fragment pathways of cyanuric acid derivatives and MRM scanning modes were explored.The ion peaks of cyanuric acid were m/z 345 215 and m/z 345 330 for qualitative and quantitative analysis,which was consistent with the ion peaks of isotopic internal standard with m/z 345215 and m/z 348217.The linear range of the developed method was between 0.010 mg/L and 0.50 mg/L and limit of detection was 0.014 mg/kg（RSN= 3）.The relative standard deviations of the developed method varied between 3.4% and 4.8% and the average recovery rates of cyanuric acid from spiked samples between 90.0% and 102.5% in the range of 0.20 mg/kg to 2.0 mg/kg.The validation results and comparison with external standard method revealed that the developed method was accurate and reliable.

关 键 词：同位素稀释质谱法 多反应监测 衍生化 三聚氰酸 乳粉 

分 类 号：O658[理学—分析化学]