摘要
目的建立同时测定结石通片中7种成分含量的一测多评(QAMS)法。方法采用高效液相色谱法,色谱柱为Waters SunFire C18柱(250 mm×4.6 mm,5μm),流动相为乙腈-0.15%甲酸水溶液(梯度洗脱),流速为1.0 mL/min,检测波长分别为330 nm(夏佛塔苷、异夏佛塔苷、异牡荆苷、绿原酸、芒果苷和大车前苷)和210 nm(茯苓酸),柱温为35℃,进样量为10μL。以绿原酸为内参物,计算其他6种成分的相对校正因子,测定含量并与外标法测定结果比较。结果夏佛塔苷、异夏佛塔苷、异牡荆苷、绿原酸、芒果苷、大车前苷和茯苓酸质量浓度分别在1.54~38.61μg/mL、0.53~13.14μg/mL、1.17~29.24μg/mL、2.05~51.28μg/mL、1.61~40.37μg/mL、1.16~29.03μg/mL、0.92~23.09μg/mL范围内与峰面积线性关系良好(r>0.9991,n=6);检测限分别为0.13,0.06,0.11,0.19,0.15,0.10,0.08μg/mL,定量限分别为0.46,0.19,0.37,0.65,0.48,0.29,0.24μg/mL,精密度、稳定性、重复性试验结果的RSD均小于2.0%(n=6);平均加样回收率分别为99.84%,98.45%,98.76%,100.35%,99.07%,99.13%,99.29%,RSD分别为1.05%,0.68%,0.98%,0.84%,1.11%,0.54%,1.26%(n=6)。夏佛塔苷、异夏佛塔苷、异牡荆苷、芒果苷、大车前苷、茯苓酸的相对校正因子分别为1.325,1.684,1.944,1.957,1.251,1.342;在不同型号仪器(不同色谱柱)、柱温条件下测定结果的RSD均小于2.0%。QAMS法与外标法7种成分含量的测定结果无显著差异(P>0.05)。结论所建立的QAMS法操作简便、结果准确,可用于结石通片多指标成分的质量控制。
Objective To establish a quantitative analysis of multi-components by single-marker(QAMS)method for the simultaneous determination of seven components in Jieshitong Tablets.Methods High-performance liquid chromatography(HPLC)method was adopted,the chromatographic column was Waters SunFire C18 column(250 mm×4.6 mm,5μm),the mobile phase was acetonitrile-0.15%formic acid aqueous solution(gradient elution),the flow rate was 1.0 mL/min,the detection wavelengths were 330 nm(schaftoside,isoschaftoside,isovitexin,chlorogenic acid,mangiferin,plantamajoside)and 210 nm(pachymic acid)respectively,the column temperature was 35℃,and the injection volume was 10μL.The relative correction factors of schaftoside,isoschaftoside,isovitexin,mangiferin,plantamajoside and pachymic acid to the internal reference chlorogenic acid were calculated,the contents were determined and compared with those determined by the external standard method(ESM).Results The linear ranges of schaftoside,isoschaftoside,isovitexin,chlorogenic acid,mangiferin,plantamajoside and pachymic acid were 1.54-38.61μg/mL,0.53-13.14μg/mL,1.17-29.24μg/mL,2.05-51.28μg/mL,1.61-40.37μg/mL,1.16-29.03μg/mL,0.92-23.09μg/mL respectively(r>0.9991,n=6).The limits of detection of the above seven components were 0.13,0.06,0.11,0.19,0.15,0.10,0.08μg/mL respectively,and their limits of quantitation were 0.46,0.19,0.37,0.65,0.48,0.29,0.24μg/mL respectively.The RSDs of precision,stability and repeatability tests were all lower than 2.0%(n=6).The average recovery rates of the above seven components were 99.84%,98.45%,98.76%,100.35%,99.07%,99.13%,99.29%respectively,with RSDs of 1.05%,0.68%,0.98%,0.84%,1.11%,0.54%,1.26%(n=6)respectively.The relative correction factors(RCFs)of schaftoside,isoschaftoside,isovitexin,mangiferin,plantamajoside and pachymic acid were 1.325,1.684,1.944,1.957,1.251 and 1.342 respectively.The RSDs of the results under different models of instruments(different chromatographic columns)and column temperatures were lower than 2.0%.There was no significant difference between the contents of seven components determined by QAMS and ESM(P>0.05).Conclusion The established QAMS method is simple and accurate,which can be used for the quality control of multi-indicator components in Jieshitong Tablets.
作者
聂溶
蔡林雪
孟倩颖
NIE Rong;CAI Linxue;MENG Qianying(The 900th Hospital of the Joint Logistics Support Force of Chinese PLA,Fuzhou,Fujian,China 350000)
出处
《中国药业》
CAS
2023年第18期85-89,共5页
China Pharmaceuticals
关键词
一测多评法
结石通片
高效液相色谱法
相对校正因子
含量测定
质量控制
quantitative analysis of multi-components by single-marker
Jieshitong Tablets
HPLC
relative correction factor
content determination
quality control
作者简介
第一作者:聂溶,女,大学本科,药师,研究方向为药物制剂分析及药理学,(电子信箱)woshinierong2022@163.com。
