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UHPLC-MS/MS法同时测定杏香兔耳风中13种成分的含量

Simultaneous determination of thirteen components in Ainsliaea fragrans by UHPLC-MS/MS
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摘要 目的建立一种快速同时测定杏香兔耳风药材中13种成分含量的UHPLC-MS/MS方法。方法采用超高效液相色谱-三重四级杆质谱技术检测,色谱柱为UPLC BEH C18(100 mm×2.1 mm,1.7μm),柱温为40℃,流动相为5 mmol甲酸铵和0.1%甲酸水溶液(A)-乙腈(B),梯度洗脱,体积流量0.25 mL/min,ESI负离子采集,雾化器和辅助气均为344.5 kPa,气帘气为206.7 kPa,喷雾电压为-4500 V,离子化温度为500℃,13种成分均采用多级反应监测模式(MRM)。结果在优化的液相-质谱条件下,原儿茶酸、咖啡酸、新绿原酸、绿原酸、隐绿原酸、1,3-二咖啡酰奎宁酸、1,5-二咖啡酰奎宁酸、3,4-二咖啡酰奎宁酸、3,5-二咖啡酰奎宁酸、4,5-二咖啡酰奎宁酸、木犀草素、木犀草苷、芹菜素的检测质量浓度线性范围分别为1.099~274.800、1.006~100.600、1.080~1080.000、83.12~8312.00、19.92~996.00、1.076~269.000、5.555~555.500、4.420~4420.000、44.76~17904.00、48.00~9600.00、2.108~210.800、4.136~413.600、1.070~107.000 ng/mL,且线性关系良好(r≥0.9958),平均加样回收率(n=6)为96.54%~99.75%,RSD为0.48%~0.96%,精密度、稳定性、重复性试验的RSD均小于3.90%。结论该方法重复性和专属性好,稳定可控,可用于杏香兔耳风药材及其制剂的质量控制。 Objective To establish an UHPLC-MS/MS method for rapid and simultaneous determination of the content of 13 components in Ainsliaea fragrans.Methods The UHPLC-MS/MS method was performed on UPLC BEH C18(100 mm×2.1 mm,1.7μm)with acetonitrile-water(containing 0.1%formic acid and 5 mmol ammonium formate)as mobile phase for gradient elution.Flow rate was 0.25 mL/min and column temperature was 40℃.A triple quadrupole mass spectrometer equipped with electrospray ionization source(ESI)was applied in negative ion mode with the following parameters:ion spray,-4500 V,ion source temperature,500℃,curtain gas,344.5 kPa,nubulizer(GS1),344.5 kPa,heater gas(GS2),206.7 kPa,and multiple reaction monitoring(MRM)was performed for quantitative analysis of these compounds.Results Under the optimized MS/MS condition,the linearity ranges of protocatechuic acid,caffeic acid,neochlorogenic acid,chlorogenic acid,cryptochlorogenic acid,1,3-dicaffeoylquinic acid,1,5-dicaffeoylquinic acid,3,4-dicaffeoylquinic acid,3,5-dicaffeoylquinic acid,4,5-dicaffeoylquinic acid,luteolin,luteoloside and apigenin were 1.099—274.800 ng/mL,1.006—100.600 ng/mL,1.080—1080.000 ng/mL,83.12—8312.00 ng/mL,19.92—996.00 ng/mL,1.076—269.000 ng/mL,5.555—555.500 ng/mL,4.420—4420.000 ng/mL,44.76—17904.00 ng/mL,48.00—9600.00 ng/mL,2.108—210.800 ng/mL,4.136—413.600 ng/mL,1.070—107.000 ng/mL(r≥0.9958),respectively,with good linearity.The average recovery rate of thirteen compounds in the samples were in the range of 96.54%—99.75%,and the RSD range was from 0.48%to 0.96%.The RSD values of precision,stability and repeatability test were all less than 3.90%.Conclusion The method had good repeatability,high specificity,stability and controllability,and could be used for quality control of A.fragrans and its preparations.
作者 吴蓓 李军茂 黄小方 姚闽 欧阳辉 何明珍 饶怡菲 冯育林 杨世林 WU Bei;LI Jun-mao;HUANG Xiao-fang;YAO Min;OUYANG Hui;HE Ming-zhen;RAO Yi-fei;FENG Yu-lin;YANG Shi-lin(Nanchang Key Laboratory of Quality and Safety Evaluation of Traditional Chinesc Medicine,Nanchang Institute for Food and Drug Control,Nanchang 330038,China;Jiangxi University of Traditional Chinese Medicine,Nanchang 330004,China;State Key Laboratory of Innovative Drug and Efficient Energy-Saving Pharmaceutical Equipment,Nanchang 330006,China;Jiangxi Institute for Drug Control,Nanchang 330029,China)
出处 《中草药》 CAS CSCD 北大核心 2020年第15期4025-4031,共7页 Chinese Traditional and Herbal Drugs
基金 国家重点研发计划“中医药现代化研究”重点专项(2019YFC1712300) 国家自然科学基金资助项目(81760702) 国家自然科学基金资助项目(81560636) 江西省卫生厅项目(2016A142) 江西省教育厅科技项目(GJJ191640) 江西中医药大学校级研究生创新专项资金项目(JZYC19)。
关键词 杏香兔耳风 质量控制 UHPLC-MS/MS 木犀草素 木犀草苷 芹菜素 原儿茶酸 咖啡酸 绿原酸 Ainsliaea fragrans Champ. quality control UHPLC-MS/MS luteolin luteoloside apigenin protocatechuic acid caffeic acid chlorogenic acids
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