摘要
目的:建立超高效液相色谱-三重四极杆质谱(UPLC-QQQ MS/MS)法测定茜草及其炮制品中遗传毒性物质芦西定和芦西定-3-O-素草苷的含量。方法:采用Waters ACQUITY UPLC BEH C_(18)(100 mm×2.1 mm,1.7μm)色谱柱,以0.1%甲酸-乙腈为流动相,梯度洗脱,体积流量0.3 mL·min^(-1),柱温30℃,进样量为1μL。采用质谱检测器,离子化模式为ESI+,多反应监测。同时以聚类分析和偏最小二乘判别分析模型对不同规格药材结果进行分析。结果:芦西定及其芦西定-3-O-素草苷在各自范围内线性关系良好(r>0.9900),平均加样回收率为99.8%和98.3%,RSD为1.1%和1.2%。生品中芦西定含量为6.51~26.28μg·g^(-1),芦西定-3-O-素草苷含量为85.77~232.73μg·g^(-1);炮制不到位茜草炭中芦西定含量为5.13~12.45μg·g^(-1),芦西定-3-O-素草苷含量为33.31~196.52μg·g^(-1);炮制到位茜草炭中芦西定含量为15.78~40.85μg·g^(-1),芦西定-3-O-素草苷含量为0~16.12μg·g^(-1)。结论:建立了茜草中芦西定和芦西定-3-O-素草苷的含量测定方法,且该方法准确稳定,重复性好,耐用性强,可以用于含量检测。炮制炒炭后遗传毒性物质芦西定和芦西定-3-O-素草苷的含量有明显差异。
Objective:To establish an ultra-performance liquid chromatography-triple quadrupole tandem mass spectrometry(UPLC-QQQ MS/MS)method for the determination of genotoxic lucidin and lucidin-3-Oprimeveroside in raw and processed Rubiae Radix et Rhizoma.Methods:The analysis was performed on a Waters ACQUITY UPLC BEH C18 column(100 mm×2.1 mm,1.7μm)using 0.1%formic acid-acetonitrile as the mobile phase in gradient elution mode.The flow rate was set at 0.3 mL·min^(-1),the column temperature was maintained at 30℃,and the injection volume was 1μL.Detection was carried out by mass spectrometry with ESI+ionization mode and multiple reaction monitoring(MRM).Additionally,the results from different grades of medicinal materials were analyzed using cluster analysis and partial least squares-discriminant analysis(PLS-DA)models.Results:Lucidin and lucidin 3-O-beta-primveroside were found to exhibit good linearity(r>0.9900)within their respective concentration ranges.The mean recovery rates were determined to be 99.8%and 98.3%with RSDs of 1.1%and 1.2%,respectively.Content of lucidin in the prepared slices were 6.51-26.28μg·g^(-1),while those of lucidin-3-O-primeveroside were 85.77-232.73μg·g^(-1).Contents of lucidin and lucidin-3-O-primeveroside in the incompletely processed Rubiae Radix et Rhizoma charcoal were 5.13-12.45μg·g^(-1),33.31-196.52μg·g^(-1).In properly processed Rubiae Radix et Rhizoma charcoal,content of lucidin were 15.78-40.85μg·g^(-1),whereas those of lucidin-3-O-primeveroside was reduced to undetectable or trace levels(0-16.12μg·g^(-1)).Conclusion:This study establishes a reliable method for quantifying lucidin and lucidin-3-O-primeveroside in Rubiae Radix et Rhizoma.The method demonstrates excellent accuracy,stability,reproducibility,and robustness,making it suitable for routine content analysis.The charcoal-processing(stir-frying)procedure significantly alters the content levels of these genotoxic substances.
作者
江凯航
张明童
黎志兵
冯学英
刘志浩
李子彬
刘东升
李冬华
马潇
JIANG Kai-hang;ZHANG Ming-tong;LI Zhi-bing;FENG Xue-ying;LIU Zhi-hao;LI Zi-bin;LIU Dong-sheng;LI Dong-hua;MA Xiao(Gansu University of Traditional Chinese Medicine,Lanzhou 730000,China;National Key Laboratory of Quality Control of Chinese Medicinal Materials and Decoction Pieces,Gansu Provincial Engineering Laboratory of Inspection and Testing Technology of Traditional Chinese and Tibetan Medicines,Gansu Institute for Drug Control,Lanzhou 730070,China;Beijing Tongrentang(Anguo)Traditional Chinese Medicine Pieces Co.,Ltd.,Anguo 071200,China)
出处
《药物分析杂志》
北大核心
2025年第4期679-685,共7页
Chinese Journal of Pharmaceutical Analysis
基金
国家药监局中药材及饮片质量控制重点实验室项目(2024GSMPA-KL13)
国家药监局中药材及饮片质量控制重点实验室项目(2022GSMPA-KL12)
国家药监局中药材及饮片质量控制重点实验室项目(2023GSMPA-KL07)
甘肃省市场监督管理局科技计划资助(SSCJG-YP-A202401)。
关键词
茜草
茜草炭
芦西定
芦西定-3-O-素草苷
含量
聚类分析
偏最小二乘判别分析(PLS-DA)
Rubiae Radix et Rhizoma
Rubiae Radix et Rhizoma charcoal
lucidin
lucidin 3-O-beta-primveroside
content
cluster analysis
partial least squares discriminant analysis(PLS-DA)
