超高效液相色谱-质谱法测定乳粉中的双氰胺

双氰胺作为乳粉中一种新出现的污染物,对人体特别是婴幼儿的健康有重要影响.本研究建立了快速、准确测定乳粉中双氰胺的超高效液相色谱-电喷雾电离质谱（UPLC-ESI/MS）分析方法.结果表明,采用含2％氨水的乙腈对乳粉样品进行萃取,同时选用UPLC BEH HILIC（150mm×2.1 mm,1.7μm）色谱柱为固定相,以10 mmol/L甲酸铵/甲酸缓冲液（pH 4.0）-乙腈为流动相,梯度洗脱,基质匹配标准曲线定量分析,可以对5～200 μg/L双氰胺样品进行快速准确测定.在ESI正离子模式下,采用选择离子监测方法进行测定时,乳粉中双氰胺的检出限为10 μg/kg.加标浓度在50,100和2...

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Bibliographic Details
Published in分析化学 Vol. 41; no. 11; pp. 1729 - 1733
Main Author 冯峰 蒋萍萍 李娜思 周洪斌 储晓刚
Format Journal Article
LanguageChinese
Published 中国检验检疫科学研究院,食品安全研究所,北京100123%华东理工大学药学院,上海,200237%镇江出入境检验检疫局综合技术中心,镇江,212008 2013
Subjects
串联质谱
乳粉
双氰胺
基质效应
超高效液相色谱
Ultra performance liquid chromatography
Tandem mass spectrometry
Milk powder
超高效液相色谱
串联质谱
基质效应
Dicyandiamide
Matrix effect
双氰胺
乳粉
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ISSN0253-3820
DOI10.3724/SP.J.1096.2013.30400

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Summary:双氰胺作为乳粉中一种新出现的污染物,对人体特别是婴幼儿的健康有重要影响.本研究建立了快速、准确测定乳粉中双氰胺的超高效液相色谱-电喷雾电离质谱（UPLC-ESI/MS）分析方法.结果表明,采用含2％氨水的乙腈对乳粉样品进行萃取,同时选用UPLC BEH HILIC（150mm×2.1 mm,1.7μm）色谱柱为固定相,以10 mmol/L甲酸铵/甲酸缓冲液（pH 4.0）-乙腈为流动相,梯度洗脱,基质匹配标准曲线定量分析,可以对5～200 μg/L双氰胺样品进行快速准确测定.在ESI正离子模式下,采用选择离子监测方法进行测定时,乳粉中双氰胺的检出限为10 μg/kg.加标浓度在50,100和200 μg/kg样品的回收率分别为83.7％,89.1％和96.7％,相对标准偏差均小于2％.本方法快捷、准确、灵敏度高,可用于乳粉中双氰胺的快速准确测定.
Bibliography:FENG Feng , JIANG Ping-Ping1 , LI Na-Si2, ZHOU Hong-Bin3 , CHU Xiao-Gang 1 1（Institute of Food Safety, Chinese Academy of Inspection and Quarantine, Beijing 100123, China） 2 （ School of Pharmacy, East China University of Science and Technology, Shanghai 200237, China） 3（ Comprehensive Technology Center, Zhenfiang Entry-Exit Inspection and Quarantine Bureau, Zhenjiang 212008, China）
Ultra performance liquid chromatography; Tandem mass spectrometry; Dicyandiamide; Milkpowder; Matrix effect
22-1125/O6
Dicyandiamide, as a new contaminant in milk powders, can lead to harmful effects to human health, especially to infants and young children. A rapid and accurate method for the determination of dicyandiamide in milk powders using ultra performance liquid chromatography-electrospray ionization-tandem mass spectrometry （UPLC-ESI-MS/MS） was established. The milk powders samples were extracted by acetonitrile which contained 2% NH4OH solution （ V/V）, the separation was carried out using an UPLC BEH HILIC（150 mm × 2.1 mm, 1
ISSN:0253-3820
DOI:10.3724/SP.J.1096.2013.30400