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.
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)
出处
《中国药事》
CAS
2023年第4期461-468,共8页
Chinese Pharmaceutical Affairs
