UPLC-TQD-MS/MS分析青海川贝母药材中的生物碱

Analysis of alkaloids in qinghai fritillaria D.Don based on UPLC-TQD-MS/MS

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.