摘要
建立了一种高效液相色谱三重四级杆质谱联用法同时测定凤香型基酒中的瓜氨酸、精氨酸的分析方法。样品氮吹、定容后,过0.22μm滤膜上机分析;以Shin-pack XR-ODSⅢ C18柱为分离柱,0.1%甲酸+2 mmol/L乙酸铵-乙腈为流动相,进行梯度洗脱,经高效液相色谱分离,在ESI正离子模式下扫描,进行多反应监测模式(MRM)检测。结果表明:在5~200μg/L范围内,瓜氨酸和精氨酸质量浓度与其峰面积线性关系良好,瓜氨酸相关系数r>0.999,精氨酸相关系数r>0.998,方法定量限为5.0μg/L。瓜氨酸和精氨酸在不同浓度下的相对标准偏差都在3.95%以下,系统精密度良好;样品平均回收率在81.7%-110.4%之间。此方法相比于常用的衍生高效液相法,样品前处理简单,检测效率高、结果准确可靠,适用于凤香型基酒中瓜氨酸、精氨酸的快速检测。
In this study,we developed a method tosimultaneously detect the Citrulline and Arginine in Fengxiang base liqquor by HPLC-MS/MS.After the sample was blown with nitrogen and constant volume,and went through 0.22μm filter membrane.Then samples were separated by Shin-pack XR-ODSⅢ C18 column,using 0.1% formic acid+2mmol/L ammonium acetate-acetonitrile as mobile phase,gradient elution by high performance liquid chromatography(HPLC)separation,scan in ESI positive ion mode for multiple reaction monitoring mode(MRM) for testing.The results showed that,in the range of 5~200μg/L,the mass concentration of citrulline and arginine had a good linear relationship with the peak area,the correlation coefficients of citrulline and arginine were respectively:r>0.999,r>0.998.And the method quantification limit was 5.0 μg/L.The relative standard deviations of citrulline and arginine at different concentrations were both below 3.95%,and the system precision was good.The average sample recovery rate was between81.7% and 110.4%.Compared with the commonly used derivatization HPLC method,this method has simple sample preparation,high detection efficiency,and accurate and reliable results.It is suitable for the rapid detection of citrulline and arginine in Fengxiang base liqquor.
作者
任璐
桑涛
刘丽丽
REN Lu;SANG Tao;LIU Lili(Shaanxi Xifeng Liquor Co..Ltd.,Baoji 721400,Shaanxi,China)
出处
《酿酒》
CAS
2022年第3期135-138,共4页
Liquor Making
关键词
高效液相色谱-质谱
凤香型基酒
瓜氨酸
精氨酸
Liquid chromatography-tandem mass spectrometry
Fengxiang base liqquor
Citrulline
Arginine
