基于UPLC-MS/MS技术的更年宁水蜜丸中藏柴胡掺伪方法的研究
Adulteration of Bupleurum marginatum var.stenophyllum in Gengnianning water-honeyed pill by UPLC-MS/MS
蒋芦荻 1杨琰 1刘亚楠 1李海燕 1王海波 1王晓燕1
作者信息
- 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,郑州 450018
- 折叠
摘要
目的 建立更年宁中藏柴胡掺伪检查方法,考察生产企业是否存在使用藏柴胡替代柴胡投料的情况.方法 采用超高效液相色谱-三重四极杆质谱联用技术,选择Waters BEH C18色谱柱(2.1 mm×50 mm,1.7 μm),流动相为乙腈(A)-0.1％甲酸水溶液(B),梯度洗脱,流速0.3 mL·min-1,柱温35 ℃,进样量1 μL;采用电喷雾离子源(ESI),负离子模式,进行多反应监测(MRM),选择 m/z 943.5 → 635.4、m/z 943.5 797.5 和 m/z 943.5 →781.5 为尼泊尔柴胡皂苷K的检测离子对.结果 尼泊尔柴胡皂苷K质量浓度在93.3～3734 ng·mL-1内与峰面积呈现良好的线性关系(r=0.9998);精密度、重复性、稳定性(24 h)试验的RSD均小于2.0％;3个浓度平均加样回收率为96.4％～99.6％(RSD均＜3.0).更年宁中藏柴胡掺伪比例在3％～100％内与尼泊尔柴胡皂苷K质量浓度的线性关系良好(r=0.9947).以掺伪藏柴胡不得过10％为限度,对44批更年宁样品进行筛查,结果5批更年宁掺伪藏柴胡22％～36％,超出拟订限度.结论 该方法准确、可靠,可用于更年宁中藏柴胡掺伪检查及市场监管.
Abstract
Objective To establish the detection method for the adulteration of Bupleurum marginatum var.stenophyllum in Gengnianning water-honeyed pill,and to find out whether Bupleurum marginatum var.stenophyllum was used to replace Bupleuri Radix in the manufacturing enterprises.Methods UPLC-MS/MS was performed on Waters BEH C18 column(2.1 mm×50 mm,1.7 μm),with acetonitrile and 0.1％formic acid as the mobile phase in gradient elution at 0.3 mL·min-1.The column temperature was 35 ℃ and the injection volume was 1 µL.A triple quadrupole mass spectrometer was used for the detection in negative ion mode with an electrospray ion source.m/z 943.5 → 635.4,m/z 943.5 → 797.5 and m/z 943.5 → 781.5 were selected as the ion pairs and multiple reaction monitoring(MRM)mode was used for the determination of nepasaikosaponin K.Results Nepasaikosaponin K showed a good linearity at 93.3～3734 ng·mL-1(r=0.9998).The RSDs of precision,repeatability and stability(24 h)were all lower than 2.0％.The average recoveries at three spiked levels were 96.4％～99.6％(RSD＜3.0％).The adulteration ratio of Bupleurum marginatum var.stenophyllum in Gengnianning water-honeyed pill showed a good linearity to the content of nepasaikosaponin K within 3％～100％(r=0.9947).Totally 44 batches of Gengnianning water-honeyed pill were screened with the limit that the doping of Bupleurum marginatum var.stenophyllum should not exceeding 10％.The doping of Bupleurum marginatum var.stenophyllum in 5 batches of Gengnianning water-honeyed pill was 22％～36％,which exceeded the proposed limit.Conclusion The method is accurate and reliable,can be used to detect the adulteration of Bupleurum marginatum var.stenophyllum in Gengnianning water-honeyed pill.
关键词
更年宁/柴胡/藏柴胡/掺伪/尼泊尔柴胡皂苷K/超高效液相色谱-质谱联用法Key words
Gengnianning water-honeyed pill/Bupleuri Radix/Bupleurum marginatum var.stenophyllum/adulteration/nepasaikosaponin K/UPLC-MS/MS引用本文复制引用
出版年
2024
NETL
NSTL
万方数据