摘要
建立了混合阴离子交换固相萃取柱净化,液相色谱串联四极杆质谱法测定婴幼儿配方食品中甲基香兰素和乙基香兰素的方法。样品经水和乙腈提取,CuSO4溶液沉淀蛋白,NaOH调节pH,增加样品溶解性,阴离子交换固相萃取柱净化。目标化合物在梯度洗脱条件下经C18柱分离后采用ESI源负离子多反应监测模式进行检测。分别选取了婴幼儿配方乳粉、米粉、果蔬泥、肉泥作为样品基质,经空白样品添加标准样品进行测试,结果表明:甲基香兰素的检出限为1～5μg/kg,乙基香兰素检出限为0.5～1μg/kg。婴幼儿配方食品中甲基香兰素平均回收率为65%～96%,RSD为3.3%～7.9%;乙基香兰素平均回收率为63%～92%,RSD为4.3%～8.2%。该方法为婴幼儿配方食品中痕量香精香料的检测和监控提供了技术支持。
A method is presented for the quantitative determination and confirmation of vanillin and ethyl vanillin in infant formulas by mixed anion-exchange solid phase extraction cartridge clean-up and liquid chromatography tandem quadrupole mass spectrometry（HPLC/MS/MS）.Acetonitrile and water were used as extraction solvents,and CuSO4 solution was used to precipitate protein in the sample.And then the solubility of the target compound was obviously improved by adjusting pH with NaOH solution.An aliquot of the supernatant was cleaned up using anion-exchange solid phase extraction cartridge.Chromatographic separation was performed on a C18 column with the gradient elution and the mass spectrometric acquisition was carried out under the ESI negative mode of multiple-reaction monitoring（MRM）.Baby formula milk powder,rice flour,fruits and vegetables mud and muddy flesh were selected as matrix spike blank samples in this test,as a result,the limits of determination（LOD） of vanillin and ethyl vanillin are 1～5 μg/kg and 0.5～1 μg/kg,respectively.The average recoveries of vanillin are from 65% to 96% with the relative standard deviations（RSDs） of 3.3%～7.9%;and the average recoveries of ethyl vanillin are from 63% to 92% with the relative standard deviations（RSDs） of 4.3%～8.2%.This method has the high sensitivity and can be applied to test and supervision of trace of aromatic chemicals added in infant formulas.
出处
《分析试验室》
CAS
CSCD
北大核心
2011年第8期84-87,共4页
Chinese Journal of Analysis Laboratory
基金
天津市质量技术监督局科技项目(10-15)资助
关键词
液相色谱
串联四极杆质谱
香兰素
婴幼儿配方食品
Liquid chromatography
Tandem quadrupole mass spectrometry
Vanillin
Infant formula
