采用亲水作用色谱-串联质谱(hydrophilic interaction chromatography-mass spectrometry,HILIC-MS/MS)建立涪城麦冬中多种氨基酸同时测定的方法。样品经水超声提取,采用乙腈、10 mmol/L乙酸铵溶液[含0.05%(体积分数)甲酸]作为流动相,用电喷雾离子源在正离子模式下进行多反应监测,对多种氨基酸的含量进行测定。结果表明,在20~5 000 ng/mL质量浓度范围内各氨基酸线性关系良好,相关系数r均大于0.995,检出限为0.41~7.7 mg/kg,回收率为81.7%~114.2%,相对标准偏差小于4.0%。因此,该测定方法提取简单,测试灵敏度高、重复性好,可有效满足涪城麦冬中多种氨基酸的同时测定。
This study aimed to establish a direct determination method of multiple amino acids in Ophiopogon japonicus by hydrophilic interaction chromatography - mass spectrometry (HILIC-MS/MS). The samples were extracted by the extraction solution of water, meanwhile, acetonitrile and 10mmol/L ammonium acetate (0.05% formic acid) were used as the mobile phase for gradient elution, multi response monitoring (MRM) of electrospray ion source under positive ions mode for quantitative determination of amino acids. Results showed that the linear relationships were good in the range of 20-5 000 ng/mL, and the correlation coefficient was greater than 0.995. Furthermore, the detection limits were 0.41-7.7 mg/kg and the average recoveries were from 81.7% to 114.2% with the relative standard deviations less than 4.0%. In conclusion, the method developed here was simple, high sensitivity and good repeatability, and can be applied to the simultaneous determination of amino acids in Ophiopogon japonicus.
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