| 固相萃取净化-微波辅助衍生-气相色谱-质谱法测定番茄酱中灭蝇胺及其代谢物三聚氰胺 |
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| 引用本文： | 李锋格,姚伟琴,田延河,李世雨,苏敏,窦辉,朱慧萍,王昭妮.固相萃取净化-微波辅助衍生-气相色谱-质谱法测定番茄酱中灭蝇胺及其代谢物三聚氰胺[J].检验检疫科学,2010,20(2):1-4,7. |
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| 作者姓名： | 李锋格 姚伟琴 田延河 李世雨 苏敏 窦辉 朱慧萍 王昭妮 |
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| 作者单位： | 新疆出入境检验检疫局,技术中心,新疆乌鲁木齐,830063 |
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| 摘 要： | 目的]建立了固相萃取净化-微波辅助衍生-气相色谱-质谱法测定番茄酱中灭蝇胺和三聚氰胺含量的分析方法。方法]样品经乙酸-乙腈-水溶液超声提取,离心,滤液经混合型阳离子交换固相萃取柱净化,氮气吹干,微波辅助硅烷化衍生,气相色谱-质谱测定,选择离子监测模式,基质匹配外标法定量。结果]在0.01～5mg/kg的范围内线性良好（r〉0.99）,在0.25～1.0mg/kg的添加水平范围内,灭蝇胺和三聚氰胺的平均回收率分别为98%～109%和84%～94%,相对标准偏差（RSD）分别为5.7%～8.5%和3.2%～7.4%,灭蝇胺和三聚氰胺的检出限（LOD）分别为0.02mg/kg和0.01mg/kg。结论]该方法简便、快速、灵敏、准确、低成本、耐用,适合番茄酱中灭蝇胺和三聚氰胺确证和定量测定。
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| 关 键 词： | 番茄酱 灭蝇胺 三聚氰胺 固相萃取 微波辅助衍生 气相色谱-质谱 |
Determination of Cyromazine and its Metabolite Melamine in Ketchup by Solid-Phase Extraction (SPE)Cleaned up-Microwave-Assisted Derivatization-Gas Chromatography-Mass Spectrometry |
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| Li Fengge,Yao Weiqin,Tian Yanhei,Li Shiyu,Su Min,Dou Hui,Zhu Huiping,Wang Zhaoni.Determination of Cyromazine and its Metabolite Melamine in Ketchup by Solid-Phase Extraction (SPE)Cleaned up-Microwave-Assisted Derivatization-Gas Chromatography-Mass Spectrometry[J].Inspection and Quarantine Science,2010,20(2):1-4,7. |
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| Authors: | Li Fengge Yao Weiqin Tian Yanhei Li Shiyu Su Min Dou Hui Zhu Huiping Wang Zhaoni |
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| Institution: | Li Fengge,Yao Weiqin,Tian Yanhei,Li Shiyu,Su Min,Dou Hui,Zhu Huiping,Wang Zhaoni(Xinjiang Entry-Exit Inspection , Quarantine Bureau,Urumqi,Xinjiang,830063) |
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| Abstract: | A solid-phase extraction(SPE) cleaned up/microwave-assisted derivatization/gas chromatography-mass spectrometry method is presented for the quantitative determination and confirmation of cyromazine and its metabolite melamine in ketchup.The ketchup sample was extracted with acetic acid-acetonitrile water solution.An aliquot of the filtrate was cleaned up using mixed-mode cation exchange solid-phase extraction(SPE) cartridges,evaporated to dryness under nitrogen gas and the residue was converted to trimethyl... |
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| Keywords: | Ketchup Cyromazine Melamine Solid-Phase Extraction(SPE) Microwave-Assisted Derivatization Gas Chromatography-Mass Spectrometry(GC-MS) |
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