浙江农业学报

• 食品科学 • 上一篇    下一篇

液相色谱—串联质谱法(LC\|MS/MS)测定固态红曲米(粉)中橘青霉素

  

  1. (浙江省农业科学院 农产品质量标准研究所,浙江 杭州 320021)
  • 出版日期:2015-05-25 发布日期:2015-05-19

Determination of citrinin in red yeast rice by LC\|MS/MS

  1. (Institute of Quality Standards for Agricultural Products, Zhejiang Academy of Agricultural Sciences, Hangzhou 310021, China)
  • Online:2015-05-25 Published:2015-05-19

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1~100 μg·L-1范围线性良好,y=6 E+07x+30800,R2=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5 μg·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。

关键词: 橘青霉素, 红曲米(粉), 液相色谱—串联质谱

Abstract: 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0 μg·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.

Key words: citrinin, red fermented rice, LC\, MS/MS