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采用稳定同位素稀释亲水作用液相色谱-串联质谱法测定婴儿配方奶粉中的双氰胺。

Determination of dicyandiamide in infant formula by stable isotope dilution hydrophilic interaction liquid chromatography with tandem mass spectrometry.

作者信息

Inoue Koichi, Sakamoto Tasuku, Min Jun Zhe, Todoroki Kenichiro, Toyo'oka Toshimasa

机构信息

Laboratory of Analytical and Bio-Analytical Chemistry, School of Pharmaceutical Sciences, University of Shizuoka, 52-1 Yada, Suruga-ku, Shizuoka 422-8526, Japan.

Laboratory of Analytical and Bio-Analytical Chemistry, School of Pharmaceutical Sciences, University of Shizuoka, 52-1 Yada, Suruga-ku, Shizuoka 422-8526, Japan.

出版信息

Food Chem. 2014 Aug 1;156:390-3. doi: 10.1016/j.foodchem.2014.01.124. Epub 2014 Feb 12.

Abstract

Dicyandiamide is a compound for reducing the negative effects of greenhouse gas emissions and nitrate leaching into waterways. In this study, the trace contamination of dicyandiamide in infant formula was analysed by stable isotope dilution hydrophilic interaction liquid chromatography with tandem mass spectrometry (HILIC-MS/MS). Dicyandiamide and a stable isotope internal standard were monitored by multiple reaction-monitoring with mass transitions: m/z 85→68/43 and m/z 89→71/45 in the electrospray positive ion mode. For sample preparation of the infant formula, a diluted/filtered procedure was developed for this assay. The calculated LOD and LOQ values were 0.01 or 0.05ng/mL for the standard solution, respectively. The averaged recovery and precision were 110.8% and 7.4%, respectively. This assay was applied to monitor 23 infant formulas, and the dicyandiamide contamination in one sample was detected and quantified at 79.1±1.2ng/g (ppb) powder. We suggest that it is necessary to cautiously monitor the DCD in common products from international countries.

摘要

双氰胺是一种用于减少温室气体排放负面影响以及硝酸盐向水道淋溶的化合物。在本研究中,采用稳定同位素稀释亲水作用液相色谱-串联质谱法(HILIC-MS/MS)分析了婴儿配方奶粉中双氰胺的痕量污染。在电喷雾正离子模式下,通过多反应监测对双氰胺和一种稳定同位素内标进行监测,其质量转移分别为:m/z 85→68/43和m/z 89→71/45。对于婴儿配方奶粉的样品制备,为此测定开发了一种稀释/过滤程序。标准溶液的计算检测限(LOD)和定量限(LOQ)分别为0.01或0.05 ng/mL。平均回收率和精密度分别为110.8%和7.4%。该测定方法应用于监测23种婴儿配方奶粉,检测并定量了一个样品中双氰胺的污染量为79.1±1.2 ng/g(ppb)粉末。我们建议有必要谨慎监测来自国际国家的常见产品中的双氰胺。

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