目的:建立养阴清肺丸中同时测定甲基麦冬黄烷酮A、甲基麦冬黄烷酮B、山麦冬皂苷B和短葶山麦冬皂苷C的分析方法,判断麦冬的投料情况。方法:应用高效液相色谱-三重四极杆串联质谱 (HPLC-MS/MS)技术,采用Agilent Poroshell 120 EC-C18(3.0 mm×100 mm,2.7μm)色谱柱, 以乙腈-0.1%甲酸溶液为流动相,流速0.3 mL·min-1,柱温35 ℃,进样量5 μL;采用电喷雾离子源 (ESI),正、负离子2种模式,以多反应监测模式(MRM)进行分析。结果:4个成分在相应的范围内线性关系良好(r>0.9991),平均回收率为96.61% ~98.65%。59批养阴清肺丸样品中有39批存在以山麦冬替代或者混入麦冬投料问题。结论:建立的方法简单、准确、可靠,可用于判断养阴清肺丸中麦冬的投料情况及市场监管。
Objective: To establish a method for the simultaneous determination of Methylophiopogonanone A, Methylophiopogonanone B, Liriopesides B and Liriopemuscari baily saponins C in Yangyin Qingfei pills and determine the feeding situation of Ophiopogonis Radix. Methods: The high performance liquid chromatographytriple quadruple mass spectrometry (HPLC-MS/MS) was performed on an Agilent Poroshell 120 EC-C18 column (3.0 mm × 100 mm, 2.7 μm) with mobile phase consisting of acetonitrileand 0.1% aqueous formic acid. The fl ow rate was controlled at 0.3 mL•min-1, and the column temperature was set at 35 ℃, and the sample volume was 5 μL. A mass spectrometer equipped with electrospray ionization source was used as detector operated in positive and negative ion mode. Multiple reaction monitoring (MRM) was performed. Results: Four components showed good linear correlation within their ranges (r>0.9991), and the averaged recoveries ranged from 96.61% to 98.65%. In the 59 batches of Yangyin Qingfei pills, 39 batches had the feeding problem of using Liriopes Radix instead of Ophiopogonis Radix or mixing in Ophiopogonis Radix. Conclusion: The established method is simple, accurate, reliable, and could be used in the determination of the feeding situation of Ophiopogonis Radix in Yangyin Qingfei pills and market regulation.
[1] 中华人民共和国药典:一部[S].2020:162.
[2] 赵佳琛,王艺涵,翁倩倩,等.经典名方中麦冬的本草考证[J].中国现代中药,2020,22(8):1381-1392.
[3] 中华人民共和国药典:一部[S].1995:19,131.
[4] 顾志荣,李芹,吕鑫,等.川麦冬、浙麦冬中8种成分测定及综合质量评价[J].中成药,2021,43(6):1513-1520.
[5] 张炜,宋文静,武嘉庚,等.UPLC-MS/MS法检测妇康宁片中掺加的山麦冬[J].中成药,2017,39(4):867-869.
[6] 谈梦霞,陈佳丽,邹立思,等.麦冬与山麦冬中多元指标成分的比较分析[J].中国中药杂志,2018,43(20):4084-4092.
[7] 王峰,何轶,于健东,等.牛黄清胃丸中麦冬掺伪情况研究[J].中国药学杂志,2019,54(16):1332-1335.
[8] 黄博,姚力,张慧,等.高分离度快速液相色谱-三重串联四极杆质谱快速检查消渴灵片中山麦冬[J].药物分析杂志,2021,41(2):320-328.
[9] 周恒,曹依敏,陈铭,等.UHPLC-MS/MS法测定坤宝丸中麦冬及其掺伪品的4种特征成分[J].中成药,2022,44(6):1929-1933.
[10] 龚雪媛,赵静芳,沈子博,等.基于HPLC-Q-TOF-MS技术检测川贝清肺糖浆中掺伪山麦冬的研究[J].海峡药学,2022,34(5):67-71.
[11] 吕轶峰,覃丽郦,白桂昌,等.石斛夜光丸中麦冬掺伪情况考察[J].中国药师,2022,25(3):550-554.
[12] 覃华亮,覃子龙,符传武.基于RRLC-QQQ-MS/MS法的清火栀麦片中4个有效成分同时测定及湖北麦冬的检查[J].药物分析杂志,2020,40(1):155-162.
[13] 单莉,魏良兵,高家荣,等.黄地安消胶囊的质量控制方法研究[J].中国药事,2015,29(5):515-521.
[14] 郭强.活血通脉片质量标准研究[J].中国药事,2014,28(12):1374-1379.
[15] 戚宝婵,曹悦,王维宁,等.养阴清肺丸质量分析[J].药物评价研究,2012,35(3):174-177.
[16] 张薇,张洁,岳峰梅.HPLC指纹图谱技术结合PLSDA在养阴清肺颗粒质量控制中的应用[J].中国药师,2021,24(2):218-222.