小儿消积止咳口服液多指标成分分析及其HPLC指纹图谱研究  

Determination of chemical constituents and quantitative fingerprints of Xiao'er Xiaoji Zhike Oral Liquid by HPLC-ESI-Q-TOF/MS

作　　者：梁琰 张贵民 苏瑞强 耿岩玲[1] 赵恒强[1] 王晓[1] 

机构地区：[1]山东省分析测试中心,山东省中药质量控制技术重点实验室,山东济南250014 [2]山东农业大学食品科学与工程学院,山东泰安271018 [3]鲁南制药集团股份有限公司,中药制药共性技术国家重点实验室,山东省中药制药新技术重点实验室,山东临沂276006

出　　处：《中草药》2017年第21期4440-4447,共8页Chinese Traditional and Herbal Drugs

基　　金：国家“十二五”科技支撑计划课题(2011BAI06B06);山东省自然科学基金资助项目(ZR2013HL029,ZR2013HM075,ZR2016YL006);山东省科技发展计划(2016GSF202014);山东省泰山学者岗位专家支持项目;山东省科学院先导项目

摘　　要：目的建立小儿消积止咳口服液(XXZOL)多指标成分分析方法及其HPLC指纹图谱,为提高其质量标准提供方法和技术支持。方法采用Agilent Zorbax SB-C18(250 mm×4.6 mm,5.0μm)色谱柱,乙腈-0.4%冰醋酸水溶液流动相体系,进行梯度洗脱,体积流量为0.6 m L/min,柱温25℃,检测波长254 nm;利用HPLC-ESI-Q-TOF/MS技术分析鉴别XXZOL中的成分,采用HPLC-DAD法对10种成分(峰1-辛弗林、峰13-绿原酸、峰16-槲皮素-3-O-β-D-葡萄糖-7-O-β-D-龙胆双糖苷、峰22-金丝桃苷、峰24-连翘酯苷A、峰26-柚皮苷、峰27-橙皮苷、峰29-新橙皮苷、峰33-连翘苷、峰37-3,29-二苯甲酰基栝楼仁三醇)进行定量测定,在多批次样品分析的基础上建立其HPLC指纹图谱。结果建立了10批样品的指纹图谱,10批样品的相似度分别为0.999 3、0.999 6、0.999 2、0.999 2、0.999 4、0.999 3、0.999 4、0.999 5、0.999 1、0.999 7,相似度均在0.9以上。XXZOL共有峰38个,确定了32个已知成分,另外有6个未知成分;10个成分量分别为2 542.42、158.61、147.02、34.35、432.42、1 813.01、1 339.70、2 580.71、175.32、1 615.17μg/m L。结论建立的XXZOL HPLC多指标成分分析及其指纹图谱,为提高其质量标准提供了科学依据。Objective To establish the HPLC multi-index quantitative fingerprints of Xiao＇er Xiaoji Zhike Oral Liquid（XXZOL）,and to provide methods and technical support for improving its quality standard.Methods Using an Agilent Zorbax SB-C18（250 mm × 4.6 mm,5.0 μm） column,acetonitrile-0.4% glacial acetic acid mobile phase system,gradient elution,flow rate of 0.6 m L/min,column temperature 25 ℃,detection wavelength 254 nm; The HPLC-ESI-Q-TOF/MS technique was used to identify the chemical constituents（peak 1-synephrine,peak 13-chlorogenic acid,peak 16-quercetin-3-O-β-D-glucose-7-O-β-D-gentiobioside,peak 22-hyperoside,peak 24-forsythoside A,peak 26-naringin,peak 27-hesperidin,peak 29-neohesperidin,peak 33-phillyrin,peak 37-3,29-dibenzoyl rarounitriol） in the XXZOL,and the content of the main components was determined by HPLC-DAD.The HPLC fingerprint was established on the basis of multi-batch analysis.Results The fingerprints of the 10 batches of samples were established,and the similarities of them were above 0.9,which were 0.999 3,0.999 6,0.999 2,0.999 2,0.999 4,0.999 3,0.999 4,0.999 5,0.999 1,and 0.999 7,respectively.XXZOL has 38 common peaks,32 of them was identified,six of them was unknown; the contents of the 10 chemical constituents were 2 542.42,158.61,147.02,34.35,432.42,1 813.01,1 339.70,2 580.71,175.32,and 1 615.17 μg/m L.Conclusion The establishment of multi-index analysis by HPLC and fingerprints of XXZOL provides a scientific basis for improving its quality standards.

关 键 词：小儿消积止咳口服液 HPLC-DAD-ESI-Q-TOF/MS 指纹图谱 多指标定量 质量标准 辛弗林 绿原酸 金丝桃苷 槲皮素-3-O-β-D-葡萄糖-7-O-β-D-龙胆双糖苷 连翘酯苷A 柚皮苷 橙皮苷 新橙皮苷 连翘苷 3 29-二苯甲酰基栝楼仁三醇 

分 类 号：R286.02[医药卫生—中药学]