摘要
建立UPLC-MS/MS测定药桑不同部位中1-脱氧野尻霉素(DNJ)含量的方法。以乙腈-0.1%的氨水为流动相,ACQUITY UPLC BEH amide(2.1×100 mm,1.7μm)为色谱柱进行分离,梯度洗脱,流速300μL·min^(-1),在串联质谱的多反应监测模式(MRM)下检测,外标法定量测定。结果表明DNJ的浓度在0.11~1.11μg·m L^(-1)范围内具有良好的线性关系(r=0.9999),加标平均回收率为100.1%,RSD≤2.0%。测得药桑葚、桑枝、桑叶中DNJ的含量分别为为0.3670%、0.0709%、1.1768%,最低检测限和定量限分别为0.2μg·kg^(-1)和0.2μg·kg^(-1)。本法具有分析速度快,无需衍生,操作方便,测定准确等优点。
A method for the determination of 1-deoxynojirimycin（ DNJ） in different parts of Morus nigra Linn.was developed by ultra high performance liquid chromatography-tandem mass spectrometry（ UPLC-MS/MS）. The UPLC-MS/MS method was performed on the ACQUITY UPLC BEH amide（ 2. 1×100 mm,1. 7 μm） column using acetonitriler -0. 1% ammonia as mobile phase with gradient elution at a flow rate of 300 μL·min^-1. The DNJ was detected under tandem mass spectrometry with multiple reaction monitoring（ MRM） mode,and quantified with external standard method. The content of DNJ had a good linear relationship within 0. 11~ 1. 11μg·m L^-1range（ r = 0. 9999）,the average recoveries were 95. 4% - 103. 5%（ RSD ≤2. 0%）. The DNJ content of fruits,leave sand branch of Morus nigra L.were 0. 3670%,0. 0709%,1. 1768%,respectively.The detection limit and quantitation limit were 0. 2 μg·kg^-1 and 0. 2 μg·kg^-1. This method had the advantage of quick analysis,without derivatization,easy operation,accurate measurement and so on.
出处
《化学研究与应用》
CAS
CSCD
北大核心
2017年第3期415-419,共5页
Chemical Research and Application
