| 引用本文: | 来灿林,侯梦妮,楼明波,孔琼荣,陈悦,朱坤丹,谢升谷,何厚洪.HPLC-Q-TOF-MS/MS分析盐酸小檗碱的杂质谱[J].中国现代应用药学,2022,39(4):512-523. |
| LAI Canlin,HOU Mengni,LOU Mingbo,KONG Qiongrong,CHEN Yue,ZHU Kundan,XIE Shenggu,HE Houhong.Analysis of Impurity Spectra of Berberine Hydrochloride by HPLC-Q-TOF-MS/MS[J].Chin J Mod Appl Pharm(中国现代应用药学),2022,39(4):512-523. |
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| HPLC-Q-TOF-MS/MS分析盐酸小檗碱的杂质谱 |
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来灿林1, 侯梦妮1, 楼明波1, 孔琼荣2, 陈悦3, 朱坤丹3, 谢升谷3, 何厚洪1
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1.浙江康恩贝制药股份有限公司药品研发中心, 杭州 310052;2.云南康恩贝希陶药业有限公司, 云南 曲靖 655000;3.浙江省食品药品检验研究院, 国家药品监督管理局仿制药评价关键技术重点实验室, 杭州 310052
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| 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-C18(4.6 mm×250 mm,5 μm),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。 |
| 关键词: 小檗碱 杂质谱 杂质质谱裂解途径 液相色谱-串联质谱法 |
| DOI：10.13748/j.cnki.issn1007-7693.2022.04.013 |
| 分类号:R917 |
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| Analysis of Impurity Spectra of Berberine Hydrochloride by HPLC-Q-TOF-MS/MS |
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LAI Canlin1, HOU Mengni1, LOU Mingbo1, KONG Qiongrong2, CHEN Yue3, ZHU Kundan3, XIE Shenggu3, HE Houhong1
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1.Drug Research and Development Center, Zhejiang Conba Pharmaceutical Co., Ltd., Hangzhou 310052, China;2.Yunnan Conba Xitao Pharmaceutical Co., Ltd., Qujing 655000, China;3.Key Laboratory of Key Technologies for Generic Drug Evaluation of the State Drug Administration, Zhejiang Institute for Food and Drug Control, Hangzhou 310052, China
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| Abstract: |
| 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-C18 (4.6 mm×250 mm, 5 μm) 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. |
| Key words: berberine impurity spectrums MS spectrum of impurity and fragmentation pathway LC-MS/MS |
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