基于HPLC-QAMS法多指标成分定量控制结合化学计量学的丹田降脂丸质量评价  

Quality evaluation of Dantian Jiangzhi pill based on HPLC-QAMS quantitative determination of multiindex components and stoichiometry

作　　者：罗玲英 廖春玲 徐晨阳 LUO Lingying;LIAO Chunling;XU Chenyang(Department of Chinese Medicine,Jiangxi Pharmaceutical School&Jiangxi Medical Technician College,Nanchang 330200,China;Department of Biomedicine,Jiangxi Pharmaceutical School&Jiangxi Medical Technician College,Nanchang 330200,China)

机构地区：[1]江西省医药学校&江西省医药技师学院中医药系,江西南昌330200 [2]江西省医药学校&江西省医药技师学院生物医药系,江西南昌330200

出　　处：《沈阳药科大学学报》2022年第12期1447-1456,共10页Journal of Shenyang Pharmaceutical University

基　　金：江西省技工院校省级教学研究重点课题(JXJGJY-ZD-201901)。

摘　　要：目的 建立高效液相一测多评法(HPLC-QAMS)同时检测丹田降脂丸中洋川芎内酯H、洋川芎内酯I、洋川芎内酯A、瑟丹酸内酯、淫羊藿苷、宝藿苷I、二氢丹参酮Ⅰ、隐丹参酮、丹参酮Ⅰ、丹参酮ⅡA的含量,并采用化学计量学方法评价丹田降脂丸的整体质量。方法 分析应用液相色谱柱Welch Ultimate XB-C_(18)(4.6 mm×250 mm, 5μm),柱温30℃。乙腈-体积分数0.2%冰醋酸溶液为流动相梯度洗脱,体积流量1.0 mL·min^(-1),检测波长280 nm。以淫羊藿苷为内参物,计算洋川芎内酯H、洋川芎内酯I、洋川芎内酯A、瑟丹酸内酯、宝藿苷I、二氢丹参酮Ⅰ、隐丹参酮、丹参酮Ⅰ及丹参酮ⅡA相对于淫羊藿苷的相对校正因子(relative correlation factor, RCF)和相对保留时间(relative retention time, RRT),利用相对校正因子计算丹田降脂丸中各成分的含量,实现一测多评;同时采用外标法(external standard method, ESM)测定10种成分的含量,并比较两者之间的差异,评价一测多评法在丹田降脂丸质量控制应用中的科学性及准确性。结果 洋川芎内酯H、洋川芎内酯I、洋川芎内酯A、瑟丹酸内酯、淫羊藿苷、宝藿苷I、二氢丹参酮Ⅰ、隐丹参酮、丹参酮Ⅰ及丹参酮ⅡA分别在0.790 0~39.50、0.960~48.00、2.690~134.5、1.070~53.50、3.280~164.0、1.360~68.00、0.430 0~21.50、0.890~44.50、1.180~59.00和1.560~78.00 mg·L^(-1)(r≥0.999 1)范围内线性关系良好。平均加样回收率及相对标准偏差(RSD)分别为96.9%(1.2%)、98.4%(1.3%)、99.7%(1.0%)、98.7%(1.2%)、100.2%(0.8%)、97.9%(0.9%)、97.7%(1.6%)、97.0%(1.0%)、97.4%(1.4%)和99.9%(0.7%)。洋川芎内酯H、洋川芎内酯I、洋川芎内酯A、瑟丹酸内酯、宝藿苷I、二氢丹参酮Ⅰ、隐丹参酮、丹参酮Ⅰ及丹参酮ⅡA相对于淫羊藿苷的RCF依次为3.238 2、2.017 5、0.913 4、1.601 1、0.955 1、3.679 6、2.147 2、1.266 7和0.851 2,各成分的校正因子和相对保留时间系统耐用性良�Objective To establish an high performance liquid chromatography-quantitative analysis of multi-components by single marker(HPLC-QAMS) method for the determination of senkyunolide H,senkyunolide I,senkyunolide A,sedanolide, icariin, baohuoside Ⅰ,15,16-dihydrotanshinone I,cryptotanshinone, tanshinone I and tanshinone IIA in Dantian jiangzhi pill, and to evaluate the consistency of the overall quality combined with chemometrics.Methods The analysis was performed on Welch Ultimate XB-C_(18) column(4.6 mm×250 mm, 5 μm),the column temperature was set at 30 ℃.The mobile phase comprised of acetonitrile-0.2% aqueous acetic acid solution flowing at 1.0 mL·min^(-1)in gradient elution.The detection wavelength were set at 280 nm.Using icariin as an internal standard, the relative conversion factor(RCF) and relative retention time(RRT) of senkyunolide H,senkyunolide I,senkyunolide A,sedanolide, baohuoside Ⅰ,15,16-dihydrotanshinone I,cryptotanshinone, tanshinone I and tanshinone IIA,The RCF was used to calculate the content of each component in Dantian jiangzhi pill, so as to achieve multiple evaluations by one test.at the same time, the content of 10 components was determined by external standard method(ESM),and the differences between the two methods were compared to evaluate the scientificity and accuracy of the HPLC-QAMS in the quality control of Dantian jiangzhi pill.Results Senkyunolide H,senkyunolide I,senkyunolide A,sedanolide, icariin, baohuoside Ⅰ,15,16-dihydrotanshinone I,cryptotanshinone, tanshinone I and tanshinone IIA showed good linear relationships within the ranges of 0.790 0-39.50,0.960-48.00,2.690-134.5,1.070-53.50,3.280-164.0,1.360-68.00,0.430 0-21.50,0.890-44.50,1.180-59.00 and 1.560-78.00 mg·L^(-1)(r≥0.999 1),whose average recoveries and relative standard deviation(RSD) were 96.9%(1.2%),98.4%(1.3%),99.7%(1.0%),98.7%(1.2%),100.2%(0.8%),97.9%(0.9%),97.7%(1.6%),97.0%(1.0%),97.4%(1.4%) and 99.9%(0.7%).The relative correction factors of senkyunolide H,senkyunolide I,senkyunolide A,sedanolide, bao

关 键 词：高效液相一测多评法 丹田降脂丸 相对校正因子 多成分 定量控制 化学计量学 

分 类 号：R917[医药卫生—药物分析学]