超高效液相色谱-质谱法评价辛芳鼻炎胶囊中柴胡投料情况  

Quality Evaluation of Bupleuri Radix in Xinfang Biyan Capsules by UPLC-MS/MS

作　　者：蒋芦荻 黄霞 李海燕 刘亚楠 茹庆国 王海波 JIANG Ludi;HUANG Xia;LI Haiyan;LIU Yanan;RU Qingguo;WANG Haibo(State Drug Administration Key Laboratory of Quality Control of Chinese Herbal Medicines and Decoction Pieces,Henan Institute for Drug and Medical Device Inspection,Zhengzhou 450018,China)

机构地区：[1]河南省药品医疗器械检验院,国家药品监督管理局中药材及饮片质量控制重点实验室,河南郑州450018

出　　处：《中国现代中药》2025年第2期328-335,共8页Modern Chinese Medicine

基　　金：2023年国家药品抽检计划(中央补助地方经费项目);国家药品监督管理局药品监管科学体系建设重点项目(RS2024Z006);国家药品监督管理局中药材及饮片质量控制重点实验室自主课题项目(ZZ202306)。

摘　　要：目的:建立超高效液相色谱-质谱法同时测定辛芳鼻炎胶囊中尼泊尔柴胡皂苷K、柴胡皂苷a和柴胡皂苷d含量的方法,评价其中藏柴胡掺伪情况和柴胡投料的质量。方法:采用Waters BEH C_(18)色谱柱(50 mm×2.1 mm,1.7μm),流动相为乙腈-0.1%甲酸水溶液,梯度洗脱,流速为0.3 m L·min^(–1),柱温为35℃,进样量为1μL;电喷雾离子源,负离子检测,多反应监测模式进行定量分析。结果:尼泊尔柴胡皂苷K、柴胡皂苷a和柴胡皂苷d对应的线性范围分别为27.6~5 527.0 ng·m L^(–1)(r=0.999 8)、124.4~24 870.0 ng·m L^(–1)(r=0.996 4)、116.6~23 318.0 ng·m L^(–1)(r=0.996 9);平均回收率分别为98.9%(RSD=1.5%)、99.5%(RSD=0.8%)、99.0%(RSD=0.7%)。47批辛芳鼻炎胶囊样品中,尼泊尔柴胡皂苷K的质量分数为0.8~54.1μg·g^(–1),柴胡皂苷a和柴胡皂苷d的总质量分数为198.5~1 321.9μg·g^(–1)。3批样品尼泊尔柴胡皂苷K的含量超出拟定限度,分别掺伪藏柴胡约54%、56%、66%;其余样品未发现掺伪或柴胡减量投料的情况。结论:建立的方法准确、可靠,可用于辛芳鼻炎胶囊中藏柴胡掺伪检查和柴胡的质量评价。Objective:This paper aims to establish an ultra high performance liquid chromatography-mass spectrometry(UPLC-MS/MS)method for the simultaneous determination of nepasaikosaponin K,saikosaponin a,and saikosaponin d in Xinfang Biyan Capsules,so as to investigate whether there is a phenomenon of using Bupleurum marginatum to replace Bupleuri Radix and evaluate the quality of Bupleuri Radix in Xinfang Biyan Capsules.Methods:C18 column(50 mm×2.1 mm,1.7μm)was used,with a mixture of acetonitrile and 0.1%formic acid as the mobile phase in gradient elution at a flow rate of 0.3 mL·min^(-1).The column temperature was 35℃,and the injection volume was 1μL.Detection was carried out in negative ion mode using an electrospray ion source(ESI).Multiple reaction monitoring(MRM)mode was employed for quantitative analysis.Results:The linear ranges of nepasaikosaponin K,saikosaponin a,and saikosaponin d were 27.6-5527.0 ng·mL^(-1)(r=0.9998),124.4-24870.0 ng·mL^(–1)(r=0.9964),116.6-23318.0 ng·mL^(-1)(r=0.9969),respectively.The average recoveries were 98.9%(RSD=1.5%),99.5%(RSD=0.8%),and 99.0%(RSD=0.7%).The contents of nepasaikosaponin K in 47 batches of Xinfang Biyan Capsule samples were 0.8-54.1μg·g^(-1).The total content of saikosaponin a and saikosaponin d was 198.5-1321.9μg·g^(-1).Three batches of samples exceeded the proposed adulteration limit of nepasaikosaponin K,and the doping of Bupleurum marginatum was 54%,56%,and 66%,respectively.There was no adulteration or low feeding of Bupleuri Radix in the other samples.Conclusion:The established method is accurate and reliable,and it can be applied to detect the Bupleurum marginatum and evaluate the quality of Bupleuri Radix in Xinfang Biyan Capsules.

关 键 词：辛芳鼻炎胶囊 柴胡 藏柴胡 掺伪 质量评价 尼泊尔柴胡皂苷K 柴胡皂苷 超高效液相色谱-质谱法 

分 类 号：R286[医药卫生—中药学]