基于HPLC-QAMS多指标成分定量控制联合化学计量学的前列安栓质量控制研究  

Quality Control of Qianliean Suppositories Based on HPLC-QAMS Multi-index Component Quantitative Control and Chemometrics

作　　者：徐晓[1] 钟贞[1] 徐凯[1] Xu Xiao;Zhong Zhen;Xu Kai(Livzon(Group)Pharmaceutical Factory,Guangdong Zhuhai 519045,China)

机构地区：[1]丽珠集团丽珠制药厂,广东珠海519045

出　　处：《中国药师》2022年第11期1944-1952,共9页China Pharmacist

基　　金：广东省工业和信息化发展专项资金(智能制造试点示范)项目(编号:粤经信创新[2017]267号)。

摘　　要：目的:建立高效液相一测多评(HPLC-QAMS)法同时检测前列安栓中虎杖苷、白藜芦醇、山栀子苷、羟异栀子苷、京尼平龙胆双糖苷、栀子苷、吴茱萸碱、吴茱萸次碱、毛冬青皂苷B_(2)、毛冬青皂苷A_(1)、毛冬青皂苷B_(1)和冬青素A的含量,并结合化学计量学方法构建其质量控制体系。方法:采用Venusil XBP C_(18)色谱柱(250 mm×4.6 mm, 5μm),流动相乙腈-0.1%磷酸,梯度洗脱;检测波长分别为290 nm(检测虎杖苷和白藜芦醇)、238 nm(检测山栀子苷、羟异栀子苷、京尼平龙胆双糖苷和栀子苷)和210 nm(检测吴茱萸碱、吴茱萸次碱、毛冬青皂苷B_(2)、毛冬青皂苷A_(1)、毛冬青皂苷B_(1)和冬青素A);以栀子苷为内参物,建立其余11种成分的相对校正因子(RCF),计算各成分含量;并运用聚类分析(CA)、主成分分析(PCA)、偏最小二乘法-判别分析(PLS-DA)和单变量分析对12种成分的相关性进行分析。结果:12种成分分别在各自范围内线性关系良好(r>0.999 0);平均加样回收率为96.98%~100.08%(RSD<2.0%);HPLC-QAMS法所测结果与外标法(ESM)差异无统计学意义(P>0.05);通过化学计量学分析,确认虎杖苷、白藜芦醇、栀子苷、吴茱萸碱、羟异栀子苷和京尼平龙胆双糖苷是影响前列安栓产品质量的差异性标志物。结论:所建立的HPLC-QAMS多指标成分定量控制及化学计量学模式识别专属性强,可用于前列安栓质量控制和综合评价。Objective:To establish an HPLC quantitative analysis of multi-components by single marker method(HPLC-QAMS)to simultaneously detect the contents of polydatin,resveratrol,shanzhiside,gardenoside,genipin 1-gentiobioside,geniposide,evodiamine,rutaecarpine,ilexsaponin B_(2),ilexsaponin A_(1),ilexoside B_(1) and ilexgenin A in Qianliean suppositories,and build its quality control system combined with chemometrics.Methods:The separation was carried out on a Venusil XBP C_(18) column(250 mm×4.6 mm,5μm).The mobile phase consisted of acetonitrile-0.1%phosphoric acid with gradient elution.The detection wavelengths were 290 nm for polydatin and resveratrol,238 nm for shanzhiside,gardenoside,genipin 1-gentiobioside and geniposide,and 210 nm for evodiamine,rutaecarpine,ilexsaponin B_(2),ilexsaponin A_(1),ilexoside B_(1) and ilexgenin A.Using geniposide as an internal standard,the relative correction factors(RCF)of the other 11 components were established and the content of each component was calculated.Cluster analysis(CA),principal component analysis(PCA),partial least squares discrimination analysis(PLS-DA)and univariate analysis were used to explore the relationships of the 12 components in Qianliean suppositories.Results:The 12 components had good linear relationships within their respective ranges(r>0.9990).The average recoveries were 96.98%-100.08%(RSD<2.0%).There was no significant difference between HPLC-QAMS and external standard method(ESM)(P>0.05).Through chemometrics analysis,polydatin,resveratrol,geniposide,evodiamine,gardenoside and genipin 1-gentiobioside were the differential markers affecting the quality of Qianliean suppositories.Conclusion:HPLC-QAMS combined with chemometric pattern recognition is specific,which can be used for the quality control and comprehensive evaluation of Qianliean suppositories.

关 键 词：前列安栓 多指标成分 高效液相一测多评法 相对校正因子 聚类分析 主成分分析 偏最小二乘法-判别分析 化学计量学 综合评价 单变量分析 

分 类 号：TQ460.72[医药卫生—药物分析学]