| 衍生化-离子阱气相色谱质谱联用检测乳粉中三聚氰胺时不同质谱检测方法研究 |
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| 引用本文： | 李东刚,鞠福龙,李春娟.衍生化-离子阱气相色谱质谱联用检测乳粉中三聚氰胺时不同质谱检测方法研究[J].化学分析计量,2009,18(2). |
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| 作者姓名： | 李东刚 鞠福龙 李春娟 |
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| 作者单位： | 黑龙江省质量监督检测研究院,哈尔滨,150050 |
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| 基金项目： | 黑龙江省科技攻关计划 |
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| 摘 要： | 利用N,O-双三甲基硅基三氟乙酰胺(BSTFA)和三甲基氯硅烷(TMCS)衍生化试剂对乳粉中三聚氰胺进行衍生化处理,利用离子阱气相色谱质谱联用仪,建立了全扫描、选择离子监测、二级质谱3种测定三聚氰胺的质谱方法.选择离子监测以三聚氰胺衍生物的特征离子m/z342,327,171,99为定性离子,以m/z327为定量离子;全扫描法二级质谱特征峰为定性依据,以特征离子m/z327为定量离子;二级质谱法以衍生物二级质谱m/z285,171,213为定性离子,以m/z 285为定量离子.3种方法的线性范围为0.05～2.0 mg/L,线性相关系数分别为0.9986、0.9990、0.9988;检测限分别为0.005、0.002、0.003 mg/kg,RSD分别为6.3%、5.7%、6.1%(n=6),方法的回收率为84%～105%.3种不同质谱检测方法应用到乳粉的检测中效果良好,均能够满足乳粉中三聚氰胺的检测要求.
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| 关 键 词： | 离子阱气相色谱质谱联用 三聚氰胺 衍生化 选择离子监测 全扫描 二级质谱 乳粉 |
DETERMINATION OF MELAMINE IN MILK POWDER BY DERIVATIVE ION TRAP GAS CHROMATOGRAPHY TANDEM MASS SPECTROMETRY WITH DIFFERENT SCAN METHODS |
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| Li Donggang,Ju Fulong,Li Chunjuan.DETERMINATION OF MELAMINE IN MILK POWDER BY DERIVATIVE ION TRAP GAS CHROMATOGRAPHY TANDEM MASS SPECTROMETRY WITH DIFFERENT SCAN METHODS[J].Chemical Analysis And Meterage,2009,18(2). |
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| Authors: | Li Donggang Ju Fulong Li Chunjuan |
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| Institution: | The Academy of Quality Inspection and Research in Heilongjiang Province;Harbin 150050;China |
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| Abstract: | With derivatization reagent BSTFA and TMCS to treatment melamine,ion trap gas chromatography tandem mass spectrometry (GC-MS-MS) was applied to determined melamine in milk powder. The method used full scan,SIM and MS/MS scan methods. GC-MS-SIM method used m/z 342,327,171,99 for qualitative ions,and used m/z 327 for quantitative ion; MS/MS method used m/z 285,171,213 for qualitative ions,used m/z 285 for quantitative ion. Linear range of three methods was 0.05-2.0 mg/L,and the correlation coefficients was 0.... |
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| Keywords: | ion trap gas chromatography tandem mass spectrometry melamine derivative SIM full scan MS/MS milk powder |
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