UPLC-MS/MS法同时测定鹤蟾片中5种成分的含量Simultaneous Determination of Five Active Components in Hechan Tablet by UPLC-MS/MS
张艳萍,钱鑫,张柳,张敏,何作民
ZHANG Yanping,QIAN Xin,ZHANG Liu,ZHANG Min,HE Zuomin
摘要(Abstract)：
目的建立同时测定鹤蟾片中贝母辛、贝母素甲、贝母素乙、华蟾酥毒基和酯蟾毒配基含量的超高效液相色谱-串联质谱(UPLC-MS/MS)法。方法采用液质联用法,应用ACQUITY UPLC BEH C_(18)柱,以乙腈-0.02 mol·L~(-1)乙酸铵水溶液为流动相,梯度洗脱,质谱采用正离子模式,多反应监测扫描。结果贝母辛、贝母素甲、贝母素乙线性范围为0.01~0.10 mg·L~(-1),华蟾酥毒基和酯蟾毒配基线性范围为0.05~0.50 mg·L~(-1),平均回收率分别为90.1%(RSD=3.6%)、102.3%(RSD=2.6%)、94.3%(RSD=3.0%)、90.7%(RSD=3.5%)、96.4%(RSD=2.5%)。结论该法操作简便、快捷、灵敏度高、能准确可靠地测定鹤蟾片中贝母辛、贝母素甲、贝母素乙、华蟾酥毒基及酯蟾毒配基5种成分的含量,可用于中成药鹤蟾片的质量控制。
OBJECTIVE To establish a UPLC-MS/MS method for the simultaneous analysis of peimisine,peimine,peiminine,cinobufagin and resibufogenin in Hechan tablet. METHODS The separation was performed on ACQUITY UPLC BEH C_(18) column using a gradient elution( acetonitrile and 0. 02 mol·L~(-1)ammonium acetate in water). A triple quadrupole mass spectrometer operating in positive electrospray ionization mode with multiple reaction monitoring was used. RESULTS The linear ranges of peimisine,peimine and peiminine,were 0.01-0.10 mg·L~(-1),cinobufagin and resibufogenin were 0.05-0.50 mg·L~(-1). The contents of five compounds were90.1%( RSD = 3.6%),102.3%( RSD = 2.6%),94.3%( RSD = 3.0%),90. 7%( RSD = 3. 5%),96. 4%( RSD = 2. 5%). CONCLUSION The method is convenient,rapid,sensitive and accurate,which can be used to separate and detect five active components peimisine,peimine,peiminine,cinobufagin and rusibufogenin in Hechan tablet.
关键词(KeyWords)：
鹤蟾片;贝母辛;贝母素甲;贝母素乙;华蟾酥毒基;酯蟾毒配基;超高效液相色谱-串联质谱法
Hechan tablet;peimisine;peimine;peiminine;cinobufagin;resibufogenin;UPLC-MS/MS
基金项目(Foundation): 广东省食药科学研究课题(2015025)
作者(Author):
张艳萍,钱鑫,张柳,张敏,何作民
ZHANG Yanping,QIAN Xin,ZHANG Liu,ZHANG Min,HE Zuomin
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