文献类型：期刊文献

中文题名：超高效液相色谱-质谱法测定乳粉中的双氰胺

英文题名：Determination of Dicyandiamide in Milk Powders Using Ultra Performance Liquid Chromatography Tandem Mass Spectrometry

作者：冯峰[1];蒋萍萍[1];李娜思[2];周洪斌[3];储晓刚[1]

机构：[1]中国检验检疫科学研究院,食品安全研究所,北京100123;[2]华东理工大学药学院,上海200237;[3]镇江出入境检验检疫局综合技术中心,镇江212008

年份：2013

卷号：41

期号：11

起止页码：1729

中文期刊名：分析化学

外文期刊名：Chinese Journal of Analytical Chemistry

收录：CSTPCD;;Scopus;WOS:【SCI-EXPANDED(收录号:WOS:000329522200014)】；北大核心:【北大核心2011】；CSCD:【CSCD2013_2014】；

基金：科技部科技支撑计划课题(No.2011BAK10B04);质检总局公益性行业科研专项项目(No.2012104002)资助

语种：中文

中文关键词：超高效液相色谱;串联质谱;双氰胺;乳粉;基质效应

外文关键词：Ultra performance liquid chromatography; Tandem mass spectrometry; Dicyandiamide; Milkpowder; Matrix effect

摘要：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.
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, 1.7μm）column, 10 mmol/L ammonium formate/formic acid buffer （pH 4.0） and acetonitrile as the mobile phases, gradient elution. The dicyandiamide was detected by ESI~ under selected ion monitoring mode. The quantified concentration range was 5- 200μg/L using matrix-matched calibration curves. When applying this method to determine real milk powder samples, the detection limits was 10μg/kg. The recoveries were 83.7% , 89.1% and 96.7% respectively when spiked negative samples with 50, 100 and 200 μg/kg dicyandiamide, and the relative standard deviations were less than 2%. This method is rapid, accurate, highly sensitive and suitable for the determination of dicyandiamide in milk powders.