感冒清热颗粒中藏柴胡检查方法的研究  

Study on the Inspection Method of Bupleurum marginatum var.stenophyllum in Ganmao Qingre Granules

作　　者：殷世宁 卢京光 宿曼筠 袁航 尹丽华 吴爱英 Yin Shining;Lu Jingguang;Su Manyun;Yuan Hang;Yin Lihua;Wu Aiying(Qingdao Institute for Food and Drug Control,NMPA Key Laboratory for Quality Research and Evaluation of Traditional Marine Chinese Medicine,Qingdao 266071,China)

机构地区：[1]青岛市食品药品检验研究院、国家药品监督管理局海洋中药质量研究与评价重点实验室,青岛266071

出　　处：《中国药事》2023年第4期461-468,共8页Chinese Pharmaceutical Affairs

摘　　要：目的:建立感冒清热颗粒中藏柴胡的检查方法,考察柴胡的掺伪情况。方法:采用液相色谱-串联质谱法,选择Agilent Poroshell 120 EC-C_(18)(100 mm×3.0 mm,2.7μm)色谱柱,以乙腈-0.1%甲酸溶液为流动相,梯度洗脱,流速0.3 mL·min^(-1),柱温35℃,进样量5μL;采用电喷雾离子源(ESI),选择m/z 943.5→797.5、m/z 943.5→781.2和m/z 943.5→635.5为尼泊尔柴胡皂苷K检测离子对,以多反应监测(MRM)模式进行测定。结果:尼泊尔柴胡皂苷K质量浓度在0.049~4.866μg·mL^(-1)范围内线性关系良好(r=0.9999),精密度、重复性良好(RSD分别为1.42%、2.24%)。以0.8μg·mL-1为掺伪判定浓度,220批感冒清热颗粒中有17批样品溶液尼泊尔柴胡皂苷K的浓度为1.2~3.5μg·mL^(-1),判定为检出藏柴胡,不合格率7.7%。结论:建立的方法准确、可靠,可用于感冒清热颗粒中柴胡的掺伪检查及市场监管。Objective:To establish the inspection method of Bupleurum marginatum var.stenophyllum in Ganmao Qingre granules and investigate the adulteration of Bupleuri Radix.Methods:The high performance liquid chromatography-tandem mass spectrometry method was performed on Agilent Poroshell 120 EC-C18(100 mm×3.0 mm,2.7μm)column,with mobile phase consisting of acetonitrile and 0.1% aqueous formic acid in gradient elution mode.The flow rate was 0.3 mL·min^(-1),the column temperature was set at 35℃ and the injection volume was 5μL.The electrospray ionization source was used as detector,m/z 943.5→797.5,m/z 943.5→781.2 and m/z 943.5→635.5 were selected as the ion pairs and multiple reaction monitoring(MRM)mode was performed for the determination of Nepasaikosaponin K.Results:Nepasaikosaponin K showed good linear relationshipin the range of 0.049-4.866μg·mL^(-1)(r=0.9999),the precision and repeatability were good,RSD were 1.42% and 2.24%,respectively,taking 0.8μg·mL^(-1) as the determination concentration for adulteration,the concentration of Nepasaikosaponin K was between 1.2 and 3.5μg·mL^(-1) of 17 samples in 220 batches of Ganmao Qingre granules,judged as the detection of Bupleurum marginatum var.stenophyllum,and the unqualified rate was 7.7%.Conclusion:The established method is accurate and reliable,and can be applied to adulteration detection of Bupleuri Radix in Ganmao Qingre granules and market regulation.

关 键 词：感冒清热颗粒 柴胡 藏柴胡 尼泊尔柴胡皂苷K 高效液相色谱-串联质谱 

分 类 号：R917[医药卫生—药物分析学]