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超高效液相色谱-串联质谱法分析贝母药材中5种生物碱
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作者单位
王文文,杨飞,杨中,范蕊,李芳,曹雪琴 1.新疆维吾尔自治区分析测试研究院2.中国科学院新疆理化技术研究所 
基金项目:新疆维吾尔自治区公益性科研院所基本科研业务经费资助项目(KYGY2016198)
中文摘要:建立了贝母药材中贝母辛、西贝母碱、贝母素乙、贝母素甲和西贝母碱苷的超高效液相色谱-串联质谱(UPLC-MS/MS )分析方法。样品经碱化甲醇-三氯甲烷提取,用Acquity UPLC BEH C18色谱柱分离,乙腈-0.1%甲酸溶液为流动相梯度洗脱,多反应监测(MRM)模式检测,外标法定量。结果表明,5种生物碱在0.000 5~0.05 mg/L范围内线性良好(r>0.999),在1.0、2.5、5.0 mg/kg加标水平下,回收率为78.6% ~93.1%,相对标准偏差不大于8.6%。5种生物碱的检出限(LOD)为0.03 mg/kg,定量下限(LOQ)为0.1 mg/kg。该方法操作简便,灵敏度高,准确可靠,适用于贝母中上述5种生物碱的同时测定。
中文关键词:贝母  生物碱  超高效液相色谱-串联质谱(UPLC-MS/MS)
 
Determination of 5 Alkaloids in Fritillaria by Ultrahigh Performance Liquid Chromatography-Tandem Mass Spectrometry
Abstract:A method of ultrahigh performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) was developed for the simultaneous determination of five alkaloids,including peimisine,sipeimine,peiminine,peimine and sipeimine 3β-D-glucoside in Fritillaria.Samples were extracted with alkaline methanol-chloroform,and separated on an Acquity UPLC BEH C18 column using acetonitrile solution containing 0.1% formic acid as mobile phase by gradient elution.The target compounds were determined by UPLC-MS/MS under multiple reaction monitoring(MRM) mode,and then quantified by external standard method.The calibration curves showed good linearities in the range of 0.000 5-0.05 mg/L with correlation coefficients(r) greater than 0.999.Recoveries for the five alkaloids at three spiked levels(1.0,2.5,5.0 mg/kg) ranged from 78.6% to 93.1%,with relative standard deviations(RSD) not more than 8.6%.The limits of detection(LOD) and limits of quantitation(LOQ) were 0.03 mg/kg and 0.1 mg/kg,respectively.The established method was simple,sensitive,accurate and reliable,and could be applied in the simultaneous determination of the five alkaloids in Fritillaria.
Key Words:Fritillaria  alkaloid  ultrahigh performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)
引用本文:王文文,杨飞,杨中,范蕊,李芳,曹雪琴.超高效液相色谱-串联质谱法分析贝母药材中5种生物碱[J].分析测试学报,2019,(4):461-465.
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