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目的建立高效液相色谱串联三重四级杆质谱法(LC-MS/MS)测定头花蓼中六种有效成分的方法。方法对样品的前处理方法及LC-MS/MS分析条件进行优化,样品以80%乙醇为提取溶剂,超声提取,LC-MS/MS多反应监测模式(MRM)用于定量测定。结果头花蓼中六种酚酸类有效成分儿茶酚、槲皮素、槲皮苷、芦丁、原儿茶酸、没食子酸能完全分离;峰面积与浓度呈良好的线性关系。添加浓度为5.0,10.0,20.0μg/kg时,六种酚酸物质的平均回收率(n=6)分别为86.90%,94.70%,85.07%,83.93%,79.33%,78.37%。RSD分别为3.51%,1.20%,2.54%,4.22%,4.68%,4.51%。结论该方法前处理简便,结果准确,重现性好,专属性高,可用于头花蓼中多种成分的含量测定和质量控制。
Objective To establish a method for the determination of six active ingredients in Polygonum capitatum by high performance liquid chromatography tandem triple-quadrupole mass spectrometry (LC-MS / MS). Methods The pretreatment method and LC-MS / MS analysis conditions were optimized. The samples were extracted with 80% ethanol, extracted by ultrasonic wave and detected by LC-MS / MS MRM. Results Polygonum capitatum in the six active phenolic compounds catechol, quercetin, quercitrin, rutin, protocatechuic acid, gallic acid can be completely separated; peak area and concentration showed a good linear relationship. The average recoveries (n = 6) of the six phenolic acids were 86.90%, 94.70%, 85.07%, 83.93%, 79.33%, 78.37% at the concentrations of 5.0, 10.0, 20.0μg / kg. RSD 3.51%, 1.20%, 2.54%, 4.22%, 4.68%, 4.51% respectively. Conclusion The method is simple, accurate, reproducible and highly specific. It can be used for the determination and quality control of various constituents in Polygonum capitatum.