摘要
使用液相色谱—串联质谱法,建立了一种萃取溶剂少、操作简单、灵敏性高,适合固态红曲米（粉）中痕量橘青霉素测定的方法。样品经甲醇提取后,以甲醇∶水（含0.1%甲酸和2 mmol·L^-1乙酸铵）体积比为90∶10作流动相在液相色谱柱上进行分离,质谱采用电喷雾源（ESI）正离子方式,选择反应监测模式（SRM）下对橘青霉素实现定性和定量分析。橘青霉素的标准品在0.1-100μg·L^-1范围线性良好,y=6 E＋07x＋30800,R^2=0.999,不同浓度添加回收试验所得样品回收率为80.9%-107.3%,方法的精密度（RSD）为2.0%,样品检测限为5μg·kg^-1。同时将该方法应用于12个从不同地域购买的红曲米（粉）产品,其中10个样品受到橘青霉素的污染,污染量为0.14-44.24 mg·kg^-1。
An analytical method was developed to determine citrinin in red yeast rice by liquid chromatography-tandem mass spectrometry （LC-MS/MS）. This method was simple, sensitive, specific, and could quantitatively detect citrinin with a small amount of extraction solvent. The samples were extracted with methanol, then the extracts were separated on a chromatographic column using methanol （containing 0. 1% formic acid and 2. 0 mmol·L^-1 ammonium acetate） ： water （90： 10, V/V） as mobile phase by gradient elution, and were finally analyzed by LC-MS/MS in selected reaction monitoring （SRM） mode via positive electrospray ionization. The method showed good linearities in the range of 0. 1 - 100 μg·kg^-1 for citrinin. The recovery rates of the different spiking concentrations were in the range of 80. 9% - 107.3%, with the relative standard deviation （RSD） of 2. 0%. The detection limits （LOD） of sample was 5.0μg·kg^-1. The proposed method was also used to determine citrinin in 12 commercial red fermented rice products from different areas. It was shown that citrinin pollution were detected in 10 samples with the level of 0. 14-44. 24 mg·kg^-1.
出处
《浙江农业学报》
CSCD
北大核心
2015年第5期841-847,共7页
Acta Agriculturae Zhejiangensis
基金
浙江省分析测试基金"基于LC-MS方法痕量检测特定农产品中的橘青霉素"(2012C37024)
