摘要
采用超高效液相色谱-串联四级杆质谱(UPLC-TQD-MS/MS)技术,建立了青海产不同基源川贝母药材中贝母素甲、贝母素乙、贝母辛和西贝母碱的分析方法。样品经超声提取,用ACQUITY UPLC BEH C18(1.7μm,2.1×100mm)色谱柱分离,乙腈-0.05%氨水为流动相梯度洗脱,在电喷雾正离子模式下,多反应监测(MRM)模式检测,外标法定量。4种生物碱在0.01~0.5μg·mL^(-1)质量浓度范围内线性良好,相关系数(r^(2))为0.9940~0.9990,4种生物碱的方法检出限(LOD S/N≥3)为0.0025μg·g^(-1),定量限(LOQ S/N=10)为0.0075μg·g^(-1),三个加标水平的回收率为71%~114%,相对标准偏差均小于10%。该方法操作简便,灵敏度高,准确可靠,适用于贝母药材中生物碱的测定。
A analytical method of ultrahigh liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)was developed for the determination of Peimine,Peiminine,Peimisine and Sipeimine in Fritillaria D.Don from different sources in Qinghai Province.The sample was extracted by ultrasound and separated by ACQUITY Beh C18(1.7 m,2.1×100 mm)column.Acetonitrile-0.05%am-monia water was gradient eluted by mobile phase.The analytes were detected by electrospray ionization mass spectrometry in posi-tive mode under multiple-reaction monitoring(MRM)mode,and quantified by external standard method.The results showed that the four alkaloids showed good linearities in the concentration range of 0.01~0.5μg·mL^(-1),with their correlation coficients(r^(2))not less than 0.9940.The limits of detection(LOD,s/n≥3)and the the limits of quantitative Limit(LOQ,s/n=10)were 0.0025μg·g^(-1)and 0.0075μg·g^(-1),respectively.The recoveries for the analytes at three spiked levels were in the range of 71%~114%,the relative standard deviation was less than 10%,The method was simple,sensitive,accurate and reliable,,and could be used for the simultaneous determination of the four alkaloids in Fritillaria.
作者
韩鸿萍
徐顺连
曹佳佳
张明锦
HAN Hong-ping;XU Shun-lian;CAO Jja-jia;ZHANG Ming-jin(School of chemistry&chemical engineering,Qinghai normal university,Xining 810008,China;The Key Laboratory ofMedicinal Plant and Animal Resources of Qinghai-Tibetan Plateau in Qinghai Province,Xining 810016,China)
出处
《化学研究与应用》
CAS
北大核心
2023年第10期2364-2369,共6页
Chemical Research and Application
基金
青海省重点研发与转化项目(2022-SF-142)资助
青海省青藏高原药用动植物资源重点实验室(2020-ZJ-Y-04)资助。
关键词
川贝母
生物碱
超高效液相色谱-串联质谱
fritillaria D.Don
alkaloids
ultrahigh liquid chromatography-tandem mass spectrometry