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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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