基于液相色谱-串联质谱法研究男宝胶囊中人参投料掺伪  

Study on the Adulteration of Panax Ginseng ET Rhizoma in Nanbao Capsules by HPLC-MS/MS

作　　者：薛平 汪嘉丽 王倬暄 李莉 刘旻虹 顾峥嵘 黄强燕 潘璐艳 XUE Ping;WANG Jiali;WANG Zhuoxuan;LI Li;LIU Minhong;GU Zhengrong;HUANG Qiangyan;PAN Luyan(Changzhou Food,Drug and Fiber Quality Supervision and Inspection Center,Changzhou 213000,China)

机构地区：[1]常州市食品药品纤维质量监督检验中心,常州213000

出　　处：《药学与临床研究》2023年第5期390-395,共6页Pharmaceutical and Clinical Research

基　　金：国家药品监督管理局2022年国家药品抽验计划(序号7)。

摘　　要：目的:采用液质联用法测定男宝胶囊中拟人参皂苷F_(11)和人参皂苷Rf的含量,其中拟人参皂苷F11是西洋参的特征成分,人参皂苷Rf是人参的特征成分,探究该制剂人参投料的概况,建立人参掺伪检测方法。方法:采用高效液相串联三重四级杆质谱仪,色谱柱为Agilent Poroshell120 SB C_(18)(2.1 mm×100 mm,2.7μm),以乙腈-水为流动相,梯度洗脱,流速0.35 mL·min^(-1),柱温40℃,进样量5μL,利用电喷雾离子源(ESI)、负离子采集模式、多反应检测模式(MRM)进行含量测定。通过模拟掺伪制备不同比例的西洋参阳性样品,从而制定合理的检测限度。结果:拟人参皂苷F11和人参皂苷Rf在线性范围内关系均良好(r≥0.9989),平均回收率分别为90.35%(RSD2.34%)和94.96%(RSD 3.50%),检测限分别为0.035μg·g^(-1)和0.028μg·g^(-1)。72批次男宝胶囊样品有1批次未检出拟人参皂苷F11,其余71批次含量范围为0.072~43.260μg·g^(-1),人参皂苷Rf 5批次未检出,67批次含量范围为1.070~34.788μg·g^(-1)。22批次样品拟人参皂苷F11含量大于拟定限度8.3μg·g^(-1)。结论:建立的检测方法简便、准确,可有效鉴别男宝胶囊中西洋参掺人参投料的问题,为此药的质量控制和市场监管提供参考。Objective:To establish a method for the simultaneous determination of pseudoginsenoside F_(11)(a characteristic component of Panacis Quinquefolii Radix)and ginsenoside Rf(a characteristic component of Panax Ginseng ET Rhizoma)in Nanbao capsules to detect adulteration.Methods:High performance liquid chromatography-triple quadruple mass spectrometry(HPLC-MS/MS)was performed on an Agilent Poroshell 120 SB C_(18)column(2.1 mm×100 mm,2.7μm).Acetonitrile-water was used as the mobile phase for gradient elution.The flow rate was controlled at 0.35 mL·min^(-1),the column temperature was set at 40℃,and the sample volume was 5μL.The mass spectrometer was equipped with an electrospray ionization source(ESI),operated in a negative ion mode and performed multiple reaction monitoring(MRM).Results:The two components showed good linearities in the selected concentration ranges(r≥0.9989).The average recovers of pseudoginsenoside F_(11) and ginsenoside Rf were 90.35%(RSD 2.34%)and 94.96%(RSD 3.50%),respectively.The detection limits were 0.035μg·g^(-1)and 0.028μg·g^(-1),respectively.One of the 72 batches of sanples did not detect pseudoginsenoside F_(11),and the content range of the rest 71 batches was 0.072-43.260μg·g^(-1).Ginsenoside Rf was not detected in 5 batches,and the content range of the other 67 batches was 1.070-34.788μg·g^(-1).The contents of pseudoginsenoside F_(11) in 22 batches of the samples were higher than the proposed limit of 8.3μg·g^(-1).Conclusion:The established method is simple and accurate,which can effectively identify the adulteration of Panacis Quinquefolii Radix into Nanbao capsules,and provide reference for the quality control and market supervision of this drug.

关 键 词：男宝胶囊 人参投料 西洋参掺伪 高效液相串联三重四级杆质谱 

分 类 号：R917[医药卫生—药物分析学]