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[摘要]
目的 建立UPLC-Q/TOF法同时定性、定量分析滇芹中主要化学成分。方法 采用超高效液相色谱串联飞行时间质谱法进行分析,色谱柱为Agilent Poroshell 120 Hilic,流动相为乙腈-0.1%甲酸水溶液,梯度洗脱,体积流量0.3 mL/min;定性、定量采用Q-TOF正负离子全扫描+IDA(信息关联采集)模式。结果 利用已建立的筛查数据库将满足质量误差小于5×10−6、同位素分布正确且含有二级碎片的离子作为分析目标化合物,结合软件Formula Finder、Mass Calculators等功能、在线数据库(Human Metabolome Database、PubChem、Chemical Book等)及二级碎片裂解规律,共鉴定出23个化合物,滇芹首次发现4个化合物。确定阿魏酸为定量分析指标性成分,其定量、定性离子分别为178和149;阿魏酸检测质量浓度线性范围为1.14~1 140 ng/mL(r=1.000),检测限、定量限分别为0.87、2.91 ng/mL,精密度、稳定性、重复性试验的RSD < 2%,加样回收率为98.13%~101.25%(RSD=1.37%,n=5)。结论 该方法灵敏度高、重现性好,分析快速、准确、可靠,可用于同时定性、定量检测滇芹药材中主要化学成分;云南滇芹中阿魏酸含量要高于西藏滇芹。
[Key word]
[Abstract]
Objective To establish UPLC-Q/TOF method for simultaneous qualitative and quantitative analysis of main chemical components in Sinodielsia yunnanensis. Methods High performance liquid chromatography tandem flight time mass spectrometry was used. Chromatographic column was Agilent shell 120 Hilic, and the flow phase was acetonitrile-0.1% acid aqueous solution (gradient elution) at a flow rate of 0.3 mL/min; Qualitative and quantitative analysis adopted Q-TOF positive anion full scanning + IDA (information correlation acquisition) mode. Results Using the established screening database, the target compounds with a mass error of less than 5×10−6, a correct isotope distribution and fragment ion are used as the target compounds. Combined with software Formula Finder, Mass Calculators and other functions, online database (Human Metabolome Database, PubChem, Chemical Book, etc.), and two stage fragmentation rule, 23 compounds were identified by qualitative identification. Ferulic acid was determined as a quantitative indicator component, and the quantitative and qualitative ions were 178 and 149, respectively; The linear range was 1.14—1 140 ng/mL (r=1.000), and the limits of detection and quantitation respectively was 0.87 ng/mL and 2.91 ng/mL; RSDs of precision, stability, and reproducibility tests were lower than 2%; The recovery rate was 98.13%—101.25% (RSD=1.37%, n=5). Conclusion This method has high sensitivity, good reproducibility, and its analysis is fast, accurate, and reliable, and it can be used for simultaneous qualitative and quantitative determination of main chemical components in the medicinal materials of S. yunnanensis; The content of ferulic acid in Yunnan is higher than that in Tibet.
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[基金项目]
国家科技重大专项(2012ZX09103201-050);重庆市科学技术委员会(cstc2017shmsA130035,cstc2017shmsA130090,cstc2017jxjl-jbky120009,cstc2017jxjl-jbky130001);重庆市卫生计生委科技项目(ZY201702142);重庆市铜梁区科技计划项目