摘要
目的采用高效液相色谱串联四级杆飞行时间质谱(HPLC-Q-TOF-MS/MS)联用技术对盐酸小檗碱杂质谱进行结构鉴定。方法采用Agilent ZORBAX SB-C_(18)(4.6 mm×250 mm,5μm),10 mmol·L^(-1)乙酸铵溶液(冰醋酸调节pH至3.0)-乙腈(75∶25)为流动相,流速为0.8 mL·min^(-1),紫外检测波长为345 nm,对小檗碱原料进行杂质分离。再采用HPLC-Q-TOF-MS/MS测定小檗碱及其杂质一级精确分子量及二级碎片离子,并进行结构解析。结果小檗碱与其杂质分离良好,植物提取原料中存在7个杂质,化学合成原料中存在5个杂质。结论液质联用技术能有效地鉴定小檗碱及其杂质结构,为质量控制提供了参考依据。
OBJECTIVE To identify the structure of berberine hydrochloride impurities by high performance liquid chromatography coupled to tandem quadrupole time-of-flight mass spectrometry(HPLC-Q-TOF-MS/MS).METHODS An Agilent ZORBAX SB-C_(18)(4.6 mm×250 mm,5μm)column was used for the separation of berberine and its impurities.The impurities of berberine were separated by the 10 mmol·L^(-1)ammonium acetate solution(adjusted pH to 3.0 with glacial acetic acid)-acetonitrile(75∶25)as the mobile phase,the flow rate was 0.8 mL·min^(-1),and the UV detection wavelength was 345 nm.The HPLC-Q-TOF-MS/MS was used to determine the precise first-order molecular weight and second-order fragment ions of berberine and its impurities,and the structure was elucidated.RESULTS Berberine and its impurities were well separated.There were 7 impurities in materials from plant extraction,and 5 impurities from chemical synthesis.CONCLUSION The LC-MS can effectively identify the structure of berberine and its impurities,providing a reference for quality control.
作者
来灿林
侯梦妮
楼明波
孔琼荣
陈悦
朱坤丹
谢升谷
何厚洪
LAI Canlin;HOU Mengni;LOU Mingbo;KONG Qiongrong;CHEN Yue;ZHU Kundan;XIE Shenggu;HE Houhong(Drug Research and Development Center,Zhejiang Conba Pharmaceutical Co.,Ltd.,Hangzhou 310052,China;Yunnan Conba Xitao Pharmaceutical Co.,Ltd.,Qujing 655000,China;Key Laboratory of Key Technologies for Generic Drug Evaluation of the State Drug Administration,Zhejiang Institute for Food and Drug Control,Hangzhou 310052,China)
出处
《中国现代应用药学》
CAS
CSCD
北大核心
2022年第4期512-523,共12页
Chinese Journal of Modern Applied Pharmacy
