摘要
目的研究白扁豆配方颗粒质量评价方法,并分析其主成分从饮片至标准汤剂及配方颗粒的含量变化。方法采用UPLC-Q-TOF/MS技术,通过对照品比对、数据库检索鉴别白扁豆配方颗粒成分;采用UPLC-ELSD法测定白扁豆配方颗粒中竹节参皂苷IVa的质量分数,以Waters CORTECS T3柱为色谱柱,柱温为25℃,流动相为0.05%甲酸溶液(A)-乙腈(B)梯度洗脱,流速为1.0 mL/min,采用ELSD检测器,其蒸发管温度为80℃,雾化温度为50℃,载气流速为1.3 L/min,进样量为7μL。结果白扁豆配方颗粒指纹图谱共标定了13个共有峰,质谱鉴别了11个成分。竹节参皂苷IVa检测质量浓度的线性范围为11.76~117.60μg/mL(r=0.9998);精密度、稳定性、重复性试验的RSD值均小于3%,竹节参皂苷IVa平均回收率为99.27%,RSD为2.68%。结论所建立白扁豆配方颗粒质量控制分析方法准确度高、专属性强、重复性好且时间较短,可用于监测白扁豆配方颗粒生产过程各阶段的质量优劣,为白扁豆配方颗粒的质量标准制定提供研究依据。
Objective To establish the qualitative and quantitative evaluation method of lablab semen album dispensing granules(LSG)and to analyze the major constituent content changes of the target component from prepared pieces(PP)to standard decoction(SD)and LSG.Methods Identification of the ingredients of LSG by database search and comparison of controls using UPLC-Q-TOF/MS technique.The content of chikusetsusaponin IVa in LSG was determined by UPLC-ELSD.The method was carried on a Waters CORTECS T3 column with temperature set at 25℃,the mobile phase consisted a mixture of 0.05%formic acid(A)and acetonitrile(B)(in gradient elution)at the flow rate of 1.0 mL/min,and the detector was ELSD.Evaporator temperature of ELSD was 80℃,the nebulizer temperature was 50℃,nitrogen carrier gas flow rate was 1.3 L/min.Injection volume was 7μL.Results A total of 13 shared peaks were set in the characteristic profile of LSG,in which 11 components were identified.The linear ranges of chikusetsusaponin IVa were 11.76-117.60μg/mL(r>0.9998).The RSDs of precision,stability and repeatability tests were all lower than 3%,and the average recovery of chikusetsusaponin IVa was 99.27%(RSD=2.68%).Conclusion The established method has the advantages of high accuracy,strong specificity,good repeatability and short time,which can be used to monitor the quality of LSG in production stage,and provide experimental reference for the foundation of quality standard of LSG.
作者
刘虹
张紫佳
LIU Hong;ZHANG Zijia(The MOE Key Laboratory for Standardization of Chinese Medicines,Shanghai University of Traditional Chinese Medicine,Shanghai 201203,China;Institute of Chinese Materia Medica,Shanghai University of Traditional Chinese Medicine,Shanghai 201203,China;Shanghai Research Center for Standardization of Traditional Chinese Medicine,Shanghai 201203,China)
出处
《现代中药研究与实践》
CAS
2023年第1期64-69,共6页
Research and Practice on Chinese Medicines
基金
国家药典委员会标准提高项目(2018Z003)
上海市自然科学基金项目(22ZR1461300)。
关键词
白扁豆配方颗粒
竹节参皂苷IVa
质量标准
含量测定
指纹图谱
Lablab semen album dispensing granules
chikusetsusaponin IVa
quality standard
content determination
characteristic fingerprint