桔贝合剂质量标准的研究和探讨  

Study and discussion on the quality standard of Jubei mixture

作　　者：李业永 LI Yongye

机构地区：[1]泰安市中医医院,山东泰安271000

出　　处：《中医临床研究》2024年第21期118-124,共7页Clinical Journal Of Chinese Medicine

摘　　要：目的:对桔贝合剂的质量标准进行研究,增加了新的检测项目和检验方法。方法:建立桔贝合剂中桔梗、枇杷叶的薄层色谱鉴别方法。建立桔贝合剂高效液相色谱特征图谱,色谱柱为Agilent ZORBAX-C18(250 mm×4.6 mm,5μm),流动相为乙腈(A)和0.1%磷酸水溶液(B),梯度洗脱,柱温30℃,流速1.0 mL/min,检测波长250 nm。建立高效液相色谱法测定桔贝合剂中贝母素甲与贝母素乙的含量,色谱柱为Waters T3 C18(250 mm×4.6 mm,5μm),流动相为乙腈–0.1%二乙胺溶液(70︰30),柱温30℃,流速1.0 mL/min,蒸发光散射检测器(ELSD)。结果:薄层色谱中样品与桔梗、枇杷叶相对应的位置特征斑点明显,分离度好;建立了以黄芩苷为参照峰的高效液相色谱特征图谱,确定了8个共有特征峰,分别来自苦杏仁、甘草、黄芩和苯甲酸钠,12批样品特征图谱与对照特征图谱的相似度大于0.95;贝母素甲和贝母素乙分别在52~520μg/mL和58~580μg/mL范围内线性关系良好,平均回收率分别为101.0%和96.3%。12批样品中贝母素甲和贝母素乙含量范围分别为12.4~55.4μg/mL和6.2~48.3μg/mL,两者含量总和范围为19.2~85.3μg/mL。结论:本研究采用薄层色谱法和高效液相色谱法,建立的检验方法可对桔贝合剂进行定性鉴别和定量测定,能够有效评价与控制桔贝合剂质量。Objective:To study the quality standard of Jubei mixture(桔贝合剂)and new test items and methods are added.Methods:The TLC methods for identification of Platycodon grandiflorum and Eriobotrya japonica in Jubei mixture were established.A HPLC specific chromatogram of the Jubei mixture was established.The HPLC test was performed in Agilent ZORBAX-C18(250 mm×4.6 mm,5μm).Gradient elution was conducted with acetonitrile(A)and 0.1%acetic acid aqueous solution(B)as the mobile phase,and the column temperature was 30℃,the flow rate was 1.0 mL/min,the detection wavelength was 250 nm.HPLC-ELSD was adopted to determine the contents of Peimine and Peiminine in Jubei mixture.The HPLC test was performed in Waters T3 C18(250 mm×4.6 mm,5μm)under the gradient elution of acetonitrile and 0.1%diethylamine aqueous solution(70:30),the column temperature was 30℃,and the flow rate was 1.0 mL/min.Results:The TLC chromatograms showed the characteristic spots were clear for the Platycodon grandiflorum and Eriobotrya japonica,and there were good separation resolutions.The characteristic fingerprints of the HPLC with Baicalin as the reference peak was established,and eight common peaks were defined,separated from bitter almond,licorice,scutellaria baicalensis and sodium benzoate,the similarities between 12 batches of samples characteristic fingerprints and the reference characteristic fingerprints were more than 0.95.The linear ranges of Peimine and Peiminine fell into 52-520μg/mL and 58-580μg/mL respectively.The mean recoveries of Peimine and Peiminine were 101.0%and 96.3%,the contents of Peimine and Peiminine in 12 batches of samples were 12.4-55.4μg/mL and 6.2-48.3μg/mL respectively,and the sum of two components was 19.2-85.3μg/mL.Conclusion:The TLC and HPLC used in this study and established methods can be used for qualitative identification and quantitative determination of Jubei mixture,and they can effectively evaluate and control the quality of Jubei mixture.

关 键 词：桔贝合剂 薄层色谱法 高效液相色谱特征图谱 贝母素甲 贝母素乙 含量 标准研究 

分 类 号：R96[医药卫生—药理学]