摘要
目的:采用超高效液相色谱-质谱法(UPLC-MS/MS)同时测定九味羌活颗粒中7个马兜铃酸类成分的含量。方法:采用Shim-pack Velox PFPP色谱柱(100 mm×2.1 mm,1.8μm),以1 mmol·L^(–1)甲酸铵溶液(含0.05%甲酸,A)-甲醇(B)为流动相梯度洗脱。体积流量为0.4 mL·min^(–1),柱温为40℃,进样量为1μL,电喷雾离子源,多反应监测模式。结果:7个马兜铃酸类成分线性关系良好,r均≥0.997,加样回收率为86.5%~112.2%;检出限为0.05~0.31 ng·mL^(–1),定量限为0.18~1.04 ng·mL^(–1)。对3个企业8批样品进行测定,结果检出马兜铃酸Ⅳa、马兜铃内酰胺的质量分数分别为0~0.417、0.021~0.173μg·g^(–1)。结论:该方法重复性好、灵敏度高,可用于九味羌活颗粒中马兜铃酸类成分的测定。
Objective:To establish an ultra high-performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS)method for the simultaneous determination of seven aristolochic acid compounds in Jiuwei Qianghuo Granules.Method:The chromatographic separation was performed on a Shim-pack Velox PFPP column(100 mm×2.1 mm,1.8μm),and gradient elution was carried out with 1 mmol·L^(–1) ammonium formate(containing 0.05%formic acid,solution A)and methanol(solution B)as the mobile phase.The column temperature was set at 40℃,and injection volume was 1μL with volumetric flow rate of 0.4 mL·min^(–1).The scanning was performed using electrospray ionization(ESI)source in multiple reaction monitoring(MRM)mode and positive ion mode.Results:The linearity of aristolochic acid components was good.The correlation coefficient of standard curve was≥0.997,and the accuracy ranged from 86.5%to 112.2%.The limits of detection were between 0.05 and 0.31 ng·mL^(–1),and the limits of quantification were between 0.18 and 1.04 ng·mL^(–1).aristolochic acidⅣa and aristololactam were detected in 8 batches of samples from three enterprises,and the mass fractions were 0-0.417μg·g^(–1) and 0.021-0.173μg·g^(–1),respectively.Conclusion:The method has good repeatability and high sensitivity,and can be used for the determination of aristolochic acids in Jiuwei Qianghuo Granules.
作者
李舒琪
孙慧珠
苏建
王常顺
石丹姝
刘永利
LI Shu-qi;SUN Hui-zhu;SU Jian;WANG Chang-shun;SHI Dan-Shu;LIU Yong-li(Hebei University of Chinese Medicine,Shijiazhuang 050200,China;Hebei Key Laboratory of Traditional Chinese Medicine Quality Evaluation and Standard Research,Hebei Institute for Drug and Medical Device Control,Shijiazhuang 050227,China;Shimadzu(China)Co.,Ltd.,Beijing,100020,China)
出处
《中国现代中药》
CAS
2024年第8期1300-1306,共7页
Modern Chinese Medicine
基金
国家药品标准制修订研究课题(2021Z16-4)
河北省重点研发计划项目(21372502D)。