感冒清热颗粒中藏柴胡掺伪检测方法的建立及掺伪限度拟定
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篇名: 感冒清热颗粒中藏柴胡掺伪检测方法的建立及掺伪限度拟定
TITLE: Establishment of the detection method for the adulteration of Bupleurum marginatum in Ganmao qingre granules and determination of adulteration limit
摘要: 目的 建立感冒清热颗粒中藏柴胡掺伪检测方法,拟定藏柴胡掺伪限度。方法采用高效液相色谱-三重四极杆质谱联用技术,采用电喷雾离子源,以多反应监测模式进行负离子扫描,以m/z943.6→635.5为定量离子对,对市售感冒清热颗粒及自制感冒清热标准样品中nepasaikosaponinK含量进行检测。同时,建立感冒清热颗粒中藏柴胡掺伪比例的计算方法,并以nepasaikosa‐poninK为指标,拟定藏柴胡掺伪限度。结果感冒清热颗粒中nepasaikosaponinK检测质量浓度的线性范围为0.051~20.200μg/mL(r=0.9991);精密度、重复性、稳定性(24h)试验的RSD均小于2.50%;平均加样回收率为97.58%(RSD=2.09%,n=9);检测限为0.60μg/g,定量限为1.80μg/g。感冒清热颗粒中藏柴胡掺伪比例在5%~100%的范围内与nepasaikosaponinK峰面积的线性关系良好(r=0.9909)。15批市售感冒清热颗粒样品中,nepasaikosaponinK的含量为2.584~56.661μg/g;1批次样品超出拟定掺伪限度(10%),不合格率为6.67%。结论所建分析方法可用于感冒清热颗粒中藏柴胡掺伪的检测,拟定掺伪限度为10%。
ABSTRACT: OBJECTIVE To establish the de tection method for the adulteration of Bupleurum marginatum in Ganmao qingre granules,and to determine the adulteration limit . METHODS HPLC-MS/MS method was used to detect the content of nepasaikosaponin K in commercial and self -made samples of Ganmao qingre granules ,using electrospray ionization ,and the analysis was carried out under multiple reaction monitoring model in negative mode with m/z 943.6→635.5 as the quantitative ion pair. The calculation method was established for the adulteration proportion of B. marginatum in Ganmao qingre granules . Taking nepasaikosaponin K as the index ,the adulteration limit was determined . RESULTS The linear range of nepasaikosaponin K were 0.051-20.200 μg/mL(r=0.999 1). RSDs of precision ,repeatability and stability (24 h)tests were all lower than 2.50%. The average recoveries were 97.58%(RSD=2.09%,n=9). The limit of detection was 0.60 μg/g,the limit of quantitation was 1.80 μg/g. The adulteration ratio of B. marginatum in Ganmao qingre granules had a good linear relationship to the peak area of nepasaikosaponin K in the range of 5%-100%(r=0.990 9). The contents of nepasaikosaponin K in 15 batches of Ganmao qingre granules were 2.584-56.661 μg/g. One batch of samples exceeded the proposed adulteration limit (10%),and the unqualified rate was 6.67%. CONCLUSIONS The established analytical method can be used to detect the adulteration of B. marginatum in Ganmao qinggre granules ,the proposed adulteration limit is 10%.
期刊: 2022年第33卷第20期
作者: 赵丹彤,高一军,毕天琛,刘靖华,朱伟堃,王素香,容蓉
AUTHORS: ZHAO Dantong,GAO Yijun,BI Tianchen,LIU Jinghua,ZHU Weikun,WANG Suxiang,RONG Rong
关键字: 感冒清热颗粒;藏柴胡;nepasaikosaponin K;掺伪;高效液相色谱-三重四极杆质谱联用技术
KEYWORDS: Ganmao qingre granules ;Bupleurum marginatum ;nepasaikosaponin K ;adulteration;HPLC-MS/MS
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