高效液相色谱-串联质谱法测定桑叶茶中1-脱氧野尻霉素的含量

Determination of 1-deoxynojirimycin in mulberry leaf tea by high performance liquid chromatography-tandem mass spectrometry

中文关键词:  桑叶茶  1-脱氧野尻霉素  高效液相色谱-串联质谱法

英文关键词:mulberry leaf tea  1-deoxynojirimycin  high performance liquid chromatography-tandem mass spectrometry

中文摘要:

      目的 建立高效液相色谱-串联质谱法检测桑叶茶中1-脱氧野尻霉素(1-deoxynojirimycin, 1-DNJ)含量的分析方法。方法 样品经70%(V/V)甲醇水超声提取, 用Xbridge amide柱(2.1 mm×100 mm, 3.5 μm)分离, 以含0.1%(V/V)甲酸溶液和乙腈作为流动相进行梯度洗脱, 采用大气压化学电离(atmosphere pressure chemical ionization, APCI)和多离子检测模式(multiple reaction monitoring, MRM)进行检测, 外标法定量。结果 目标物在0.01~0.2 mg/L范围内线性相关系数大于0.99; 1-脱氧野尻霉素的定量限为5 mg/kg; 在5~50 mg/kg浓度范围内加标回收实验, 平均回收率为94.2%~98.7%, 相对标准偏差为3.2%~4.7%。结论 该方法具有分析速度快、操作简便等优点, 可用于桑叶茶中1-脱氧野尻霉素的含量测定。

英文摘要:

      Objective To establish a method for the determination of 1-deoxynojirimycin (1-DNJ) in mulberry leaf tea by high performance liquid chromatography-tandem mass spectrometry. Methods Samples were extracted with 70% (V/V) methanol solution. The liquid was performed on Xbridge amide column (2.1 mm×100 mm, 3.5 μm) with the gradient elution of 0.1% (V/V) formic acid aqueous solution and acetonitrile solution. The sample was detected by atmosphere pressure chemical ionization (APCI) using multiple reactions monitoring mode (MRM), and quantified by external standard method. Results Within the range of 0.01–0.2 mg/L, the correlation of linear was above 0.99. The limit of quantitative of the method was 5 mg/kg. The average recoveries were 94.2%–98.7% and the relative standard deviations were 3.2%–4.7% in the concentration range of 5–50 mg/kg. Conclusion This method is simple and rapid, which is suitable for the determination of 1-deoxynojirimycin in mulberry leaf tea.