基于UPLC-MS/MS吴茱萸不同炮制品种的有效成分含量测定及多元统计分析  

Content Determination and Multivariate Statistical Analysis of Effective Ingredients in Different Processed Products of Wuzhuyu(Euodiae Fructus)

作　　者：赵文燕 张安然 王蝉 向茜 杨嵩虹[1] 于欢[1] 龚千锋[1] ZHAO Wenyan;ZHANG Anran;WANG Chan;XIANG Qian;YANG Songhong;YU Huan;GONG Qianfeng(College of Pharmacy,Jiangxi University of Traditional Chinese Medicine,Nanchang 330004,Jiangxi,China)

机构地区：[1]江西中医药大学药学院,江西南昌330004

出　　处：《中华中医药学刊》2023年第3期181-185,I0028,共6页Chinese Archives of Traditional Chinese Medicine

基　　金：国家中药管理局标准化建设项目(ZYBZH-Y-JX-27)。

摘　　要：目的建立超高效液相色谱-串联质谱(UPLC-MS/MS)同时测定吴茱萸生品及不同炮制品中10种成分的含量,并结合多元统计分析方法研究其差异性,以期建立能够快速区分吴茱萸不同制法所得饮片的方法。方法采用色谱柱为Titank C18(2.1 mm×100 mm,1.8μm),柱温为40℃,流速为0.3 mL·min^(-1),正离子模式下以0.1%甲酸水溶液(A)-0.1%甲酸乙腈溶液(B)为流动相,负离子模式下以0.1%甲酸水溶液(A)-乙腈(B)为流动相,进行梯度洗脱;质谱采用ESI离子源正负离子扫描,以多反应监测模式(MRM)进行检测;对吴茱萸生品及不同炮制品中该10种成分的含量测定结果进行聚类分析和主成分分析,评价其质量差异性,进而对本分类方法进行归纳总结。结果10种成分在相应的质量浓度范围内线性关系良好,r≥0.9990,平均加样回收率为96.60%~102.37%,RSD均小于3%,精密度、稳定性、重复性试验的RSD均小于3%。定量测定结果显示吴茱萸生品与炮制品在多种成分上存在一定的差异,整合多元统计分析均可明显区分生品与不同炮制品。结论研究建立了一种能高效快速测定10种成分含量的方法,同时灵敏度高,重复性和专属性好,整合多元统计分析方法后可有效区分吴茱萸生品与不同炮制品,为吴茱萸不同饮片的鉴别及质量分析工作提供一定的科学参考。Objective To establish the ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)to simultaneously determine the contents of 10 components in Wuzhuyu(Euodiae Fructus)raw products and different processed products,and combined with multivariate statistical analysis methods to study their differences.Methods The column was Titank C18(2.1 mm×100 mm,1.8μm).The positive ion mode used 0.1%formic acid aqueous solution(A)-0.1%formic acid acetonitrile solution(B)as the mobile phase,and the negative ion mode used 0.1%formic acid aqueous solution(A)-Acetonitrile(B)as the mobile phase gradient elution.The column temperature was 40℃and the flow rate was 0.3 mL·min-1.The mass spectrometer was scanned by ESI ion source positive and negative ions and detected by the multiple reaction monitoring mode(MRM).Principal component analysis and cluster analysis were performed on the content determination results of products and different processed products to evaluate their quality differences.Results Ten components had a good linear relationship in the corresponding mass concentration range,r≥0.999.The average sample recovery rate was 96.60%to 102.37%,the RSD was less than 3%,and the RSD of the precision,stability and repeatability tests were all less than 3%.The quantitative determination results showed that there was a certain difference between the raw and processed products of Wuzhuyu(Euodiae Fructus),and the multivariate statistical analysis can clearly distinguish the raw and processed products.Conclusion The method established in this study is efficient,fast,sensitive,repeatable and specific,and can effectively distinguish the raw and processed products of Wuzhuyu(Euodiae Fructus),and provide a reference for the identification and quality analysis of the raw and processed products of Wuzhuyu(Euodiae Fructus).

关 键 词：吴茱萸 含量测定 UPLC-MS/MS 整合多元统计分析 炮制 

分 类 号：R284.1[医药卫生—中药学]