论文部分内容阅读
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 an ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS / MS) method for the simultaneous determination of Fombaxin, Fritillaria, Fritillaria, . Methods LC-MS was performed on a ACQUITY UPLC BEH C 18 column using a mobile phase of acetonitrile-0.02 mol·L -1 ammonium acetate as mobile phase with gradient elution. The mass spectra were analyzed by positive ion mode, . Results The linear ranges of Fosamprenate, Fritillariae and Peiminine were 0.01-0.10 mg · L -1. The linear ranges of Cinobufagin and Resibufogenin were 0.05-0.50 mg · L ~ (-1) -1). The average recoveries were 90.1% (RSD = 3.6%), 102.3% (RSD = 2.6%), 94.3% (RSD = 3.0%), 90.7% 2.5%). Conclusion The method is simple, rapid and sensitive. It can accurately and reliably determine the contents of Fosamil, Fritillaria, Fritillaria and Sapogenin in Crane toad tablets, Can be used for quality control of Chinese medicine Tsurumappan tablets.