HPLC-Q-TOF-MS/MS分析盐酸小檗碱的杂质谱

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。

Analysis of Impurity Spectra of Berberine Hydrochloride by HPLC-Q-TOF-MS/MS

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.