蛤蚧定喘丸中麦冬掺伪山麦冬鉴别方法建立  

Establishment of Identification Method for the Adulteration of Ophiopogonis Radix with Liriopes Radix in Gejie Dingchuan Pills

作　　者：张瑾 周煜 华小懿 浦洁 ZHANG Jin;ZHOU Yu;HUA Xiaoyi;PU Jie(Wuxi Center for Drug Safety Control,Wuxi,Jiangsu,China 214000)

机构地区：[1]江苏省无锡市药品安全检验检测中心,江苏无锡214000

出　　处：《中国药业》2025年第5期62-67,共6页China Pharmaceuticals

基　　金：国家药品监督管理局2022年国家药品抽验计划[中检监督函[2022]65号]。

摘　　要：目的 建立鉴别蛤蚧定喘丸中麦冬掺伪品山麦冬的超高效液相色谱-四极杆-静电场轨道阱高分辨质谱(UPLC-Q-Exactive MS)法。方法 色谱柱为Agilent Poroshell 120 SB-C_(18)柱(100 mm×2.1 mm,2.7μm),流动相为乙腈-0.1%甲酸溶液(50∶50,V/V),流速为0.3 mL/min,柱温为35℃,进样量为3μL,采用电喷雾正离子(ESI~+)模式,以平行反应监测(PRM)模式扫描。结果 甲基麦冬黄烷酮A、甲基麦冬黄烷酮B、山麦冬皂苷B、短葶山麦冬皂苷C的质量浓度分别在0.049~1.234μg/mL、0.049~1.235μg/mL、2.038~50.960μg/mL、2.136~53.410μg/mL范围内与峰面积线性关系良好(r≥0.999 0,n=5);检测限分别为0.007,0.007,0.061,0.320 ng;精密度、稳定性、重复性试验结果的RSD均小于3.0%(n=6);平均加样回收率分别为92.62%,96.50%,95.64%,97.18%,RSD分别为2.08%,2.43%,2.11%,2.17%(n=6)。51批蛤蚧定喘丸中,有9批检出山麦冬皂苷B,表明存在混入山麦冬投料情况。结论 所建立的方法快速、准确、可靠,可用于判断蛤蚧定喘丸中麦冬的投料情况,也可为其他含麦冬制剂中掺伪山麦冬的监测提供参考。Objective To establish an ultra-high performance liquid chromatography-quadrupole-electrostatic field orbital trap high-resolution mass spectrometry(UPLC-Q-Exactive MS)method for identifying the adulteration of Ophiopogonis Radix with Liriopes Radix in Gejie Dingchuan Pills.Methods The chromatographic column was Agilent Poroshell 120 SB-C18 column(100 mm×2.1 mm,2.7μm),the mobile phase was acetonitrile-0.1%formic acid solution(50∶50,V/V),the flow rate was 0.3 mL/min,the column temperature was 35℃,the injection volume was 3μL,and the electrospray positive ion(ESI+)mode was adopted with parallel reaction monitoring(PRM)mode for scanning.Results The linear ranges of methylophiopogonanone A,methylophiopogonanone B,liriopeside B,and liriope muscari baily saponins C were 0.049-1.234μg/mL,0.049-1.235μg/mL,2.038-50.960μg/mL,and 2.136-53.410μg/mL,respectively(r≥0.9990,n=5).The limits of detection were 0.007,0.007,0.061,and 0.320 ng,respectively.The RSDs of precision,stability,and repeatability test results were all lower than 3.0%(n=6).The average recoveries of methylophiopogonanone A,methylophiopogonanone B,liriopeside B,and liriope muscari baily saponins C were 92.62%,96.50%,95.64%,and 97.18%,with RSDs of 2.08%,2.43%,2.11%,and 2.17%,respectively(n=6).Among the fifty-one batches of Gejie Dingchuan Pills,nine batches were found to contain liriopesides B,indicating the presence of the feeding problem of mixing Liriopes Radix in Ophiopogonis Radix.Conclusion The established method is fast,accurate,and reliable,and can be used to determine the feeding status of Ophiopogonis Radix in Gejie Dingchuan Pills.It can also provide a reference for monitoring of adulterated Liriopes Radix in other preparations containing Ophiopogonis Radix.

关 键 词：蛤蚧定喘丸 超高效液相色谱-四极杆-静电场轨道阱高分辨质谱法 麦冬 山麦冬 

分 类 号：R932[医药卫生—生药学] R284.1[医药卫生—药学] R286.0