Page 59 - 《中国药房》2021年20期
P. 59

HPLC-一测多评法同时测定壮药罗汉茶中 6 种黄酮类成分及多

        元统计分析             Δ


              *
        燕 霞 ,朱雪妍 ,何颂华,张 慧,罗 轶,黄清泉(广西壮族自治区食品药品检验所/国家药品监督管理局中药
                       #
        材质量监测与评价重点实验室,南宁 530021)

        中图分类号 R284          文献标志码 A          文章编号 1001-0408(2021)20-2485-07
        DOI  10.6039/j.issn.1001-0408.2021.20.09
        摘  要   目的:建立同时测定罗汉茶中新落新妇苷、落新妇苷、新异落新妇苷、异落新妇苷、槲皮苷和黄杞苷含量的方法,并进行多
        元统计分析。方法:采用高效液相色谱-一测多评法。色谱柱为Phenomenex SuperLu C18,流动相为乙腈-0.1%甲酸溶液(19∶81,V/V),
        检测波长分别为254 nm(新落新妇苷、落新妇苷、新异落新妇苷、异落新妇苷、黄杞苷)、291 nm(槲皮苷),流速为1.0 mL/min,柱温
        为30 ℃,进样量为10 μL。以落新妇苷为内参物,计算其他5种成分的相对校正因子,再根据相对校正因子计算各成分的含量,并
        与外标法进行比较;采用SPSS 22.0软件进行聚类分析和主成分分析。结果:新落新妇苷、落新妇苷、新异落新妇苷、异落新妇苷、
        槲皮苷和黄杞苷检测进样量的线性范围分别为 0.007~0.311、0.871~18.184、0.002~0.119、0.052~1.251、0.105~2.202、0.020~
        2.319 μg(r>0.999);精密度、重复性、稳定性(24 h)试验的 RSD 均小于 3%;平均加样回收率分别为 97.32%、94.89%、97.15%、
        96.90%、97.52%、97.53%(RSD为1.09%~2.60%,n=6)。新落新妇苷、新异落新妇苷、异落新妇苷、槲皮苷、黄杞苷相对于落新妇
        苷的平均相对校正因子分别为1.252 6、1.198 3、0.958 6、0.807 1、1.138 1。一测多评法测得新落新妇苷、新异落新妇苷、异落新妇
        苷、槲皮苷、黄杞苷等 5 种成分的含量分别为 0.394 2~2.067 2、0.139 1~0.804 7、2.864 8~8.554 8、4.581 2~11.371 1、1.028 9~
        13.401 5 mg/g;外标法测得新落新妇苷、落新妇苷、新异落新妇苷、异落新妇苷、槲皮苷和黄杞苷等6种成分的含量分别为0.367 2~
        1.925 3、46.361 1~126.342 1、0.138 1~0.798 8、2.966 2~8.857 8、4.642 5~11.523 3、0.970 6~12.641 9 mg/g;两种方法含量测定结
        果的相对误差均不高于3.55%。聚类分析结果显示,9批罗汉茶样品可聚为两类,S8聚为一类、其余聚为一类。主成分分析结果
        显示,前2个主成分的累计方差贡献率为84.745%,分类结果与前者一致。结论:所建高效液相色谱-一测多评法准确、可行,重复
        性良好,可用于罗汉茶中6种黄酮类成分的同时测定,并可为其质量控制提供参考。
        关键词 罗汉茶;高效液相色谱法;一测多评法;黄酮;含量;聚类分析;主成分分析

        Simultaneous Determination of 6 Flavonoids in Zhuang Medicine Engelhardia roxburghiana by
        HPLC-QAMS and Multivariate Statistical Analysis
        YAN Xia,ZHU Xueyan,HE Songhua,ZHANG Hui,LUO Yi,HUANG Qingquan(Guangxi Zhuang Autonomous
        Region Institute for Food and Drug Control/NMPA Key Laboratory for Quality Monitoring and Evaluation of
        Traditional Chinese Medicine,Nanning 530021,China)

        ABSTRACT OBJECTIVE:To establish a method for simultaneous determination of neoastilbin,astilbin,neoisoastilbin,isoastilbin,
        quercitrin and engeletin in Engelhardia roxburghiana,and conduct multivariate statistical analysis. METHODS:HPLC-QAMS
        method was adopted. The determination was performed on Phenomenex SuperLu C18 column with mobile phase consisted of
        acetonitrile-0.1% formic acid (19 ∶ 81,V/V) at the flow rate of 1.0 mL/min. The detection wavelengths were set at 254 nm
       (neoastilbin,astilbin,neoisoastilbin,isoastilbin,engeletin)and 291 nm(quercitrin). The column temperature was 30 ℃,and
        sample size was 10 μL. Using astilbin as internal substance,and the relative correction factors of other 5 factors were calculated.
        The contents of each component were calculated according to relative correction factor,and were compared with the results of
        external standard method. SPSS 22.0 software was used for cluster analysis and principal component analysis. RESULTS:The
        linear range of neoastilbin,astilbin,neoisoastilbin,isoastilbin,quercitrin and engeletin were 0.007-0.311,0.871-18.184,0.002-0.119,
        0.052-1.251,0.105-2.202,0.020-2.319 μg(r>0.999),respectively. RSDs of precision,reproducibility and stability(24 h)tests
        were all lower than 3%. The average recoveries were 97.32%,94.89%,97.15%,96.90%,97.52% and 97.53%(RSDs were
                                                           1.09% -2.60% ,n=6),respectively. The relative correction
           Δ 基金项目:广西科技计划项目(No.桂科 AB17292069);广西药
                                                           factors of neoastilbin,neoisoastilbin,isoastilbin,quercitrin and
        品监督管理局科研计划(No.桂药科2019-12);南宁市科学研究与技术
                                                           engeletin were 1.252 6,1.198 3,0.958 6,0.807 1 and 1.138 1,
        开发计划(No.20191035)
           *主管药师,硕士。研究方向:药品质量标准。E-mail:357833410@          respectively. The contents of neoastilbin, neoisoastilbin,
        qq.com                                             isoastilbin,quercitrin and engeletin measured by QAMS were
           # 通信作者:副主任药师,硕士。研究方向:中药民族药质量标                   0.394 2-2.067 2,0.139 1-0.804 7,2.864 8-8.554 8,4.581 2-
        准。电话:0771-5827218。E-mail:384500662@qq.com          11.371 1,1.028 9-13.401 5 mg/g;the contents of neoastilbin,


        中国药房    2021年第32卷第20期                                            China Pharmacy 2021 Vol. 32 No. 20  ·2485 ·
   54   55   56   57   58   59   60   61   62   63   64