摘要
目的:通过超高效液相串联质谱(UPLC-MS/MS)方法测定番泻叶中吡咯里西啶生物碱(PA)的含量,为番泻叶的安全评估奠定基础。方法:以95%甲醇水为溶剂对番泻叶药材进行超声提取,阳离子交换固相萃取小柱净化富集。采用ZorbaxEclipsePlusC18(150mm×3.0mm,1.8μm)色谱柱,流动相为甲醇-水-0.1%甲酸,梯度洗脱,流速为0.4mL·min^-1;电喷雾离子源,正离子多反应监测模式。结果:14个PA化合物具有较好的线性关系(r>0.9905),各化合物回收率为80.60%~103.22%,精密度和准确度良好,方法检出限和定量限分别为0.1~0.5、0.2~1.0μg·L^-1。从12批番泻叶主要检测出5种PA,且PA的总质量分数为7.06~187.97μg·kg^-1。根据最高日摄入量计算,5批番泻叶药材中的PA摄入量超过0.42μg·d^-1。结论:本研究首次通过UPLC-MS/MS检测到了番泻叶中的PA,通过对其日摄入量的分析,为番泻叶的安全评价提供参考。
Objective:To lay a foundation for the safety assessment of Sennae Folium,ultra-high performance liquid chromatography-triple quadrupole tandem mass spectrometry (UPLC-MS/MS )method was used for the determination of pyrrolizidine alkaloids (PA )in Sennae Folium. Methods:These samples were extracted with 95% methanol by ultrasonic method and purified using cation exchange solid-phase extraction.The detection was performed on a Zorbax Eclipse Plus C 18 column ( 3.0 mm ×150 mm,1.8 μm ),together with the mobile phase consisted of 0.1% formic acid in methanol and 0.1% formic acid in water.The flow rate was 0.4 mL · min^-1 in a gradient elution manner.Ion source was electrospray ion source,scanning mode was MRM m ode and positive ion mode monitoring was adopted. Results:14 compounds showed good linearity ( r>0.990 5 ). The average recoveries rate of each compound were from 80.60% to 103.22%.Satisfactory precision and accuracy were obtained .Limit of detection and limit of quantitation ranged from 0.1 to 0.5 μg · L^-1 and from 0.5 to 1.0 μg · L^-1 ,respectively. 5 PA were mainly detected from 12 batches of samples and the total contents of PA varied from 7.06 to 187.97 μg · kg^-1 . Conclusion :In this study,PA in Sennae Folium was detected by UPLC-MS/MS method for the first time,and provide certain basis for the safety evaluation via the analysis of its daily intake.
作者
陈丽华
王钧篪
乔月
王慧娟
沈连钢
廖永红
孙迪安
斯建勇
CHEN Li-hua;WANG Jun-chi;QIAO Yue;WANG Hui-juan;SHEN Lian-gang;LIAO Yong-hong;SUN Di-an;SI Jian-yong(Key Laboratory of Bioactive Substances and Resources Utilization of Chinese Herbal Medicine,Ministry of Education, Institute of Medicinal Plant Development,Chinese Academy of Medical Sciences & Peking Union Medical College, Beijing 100193,China)
出处
《中国现代中药》
CAS
2019年第7期931-936,共6页
Modern Chinese Medicine
基金
中国医学科学院医学与健康科技创新工程(2017-I2M-1-013)
