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目的:用HPLC-ESI-MSn法分离和鉴定国产盐酸克林霉素棕榈酸酯原料药中的10种杂质,并探讨这些杂质的质谱裂解规律。方法:采用Agilent ZORBAX SB-C8色谱柱(150 mm×3.0 mm,3.5μm),流动相为5 mmol.L-1醋酸铵溶液-乙腈(25∶75),在正离子检测方式下,AB SCIEX 4000 Q TRAP LC/MS/MS仪对盐酸克林霉素棕榈酸酯中的杂质进行在线多级质谱分析。结果:通过多级质谱裂解推断盐酸克林霉素棕榈酸酯原料药中10种杂质分别为克林霉素、丙叉克林霉素、亚砜克林霉素棕榈酸酯、克林霉素十二酸酯、棕榈酸乙酯、克林霉素十四酸酯、克林霉素B棕榈酸酯、表克林霉素棕榈酸酯、克林霉素十八酸酯、丙叉克林霉素棕榈酸酯。结论:鉴定了盐酸克林霉素棕榈酸酯原料药中10个杂质的结构,其中3个杂质为新的杂质。
OBJECTIVE: To isolate and identify 10 kinds of impurities in clindamycin hydrochloride palmitate hydrochloride by HPLC-ESI-MSn and to explore the mass spectrometry cleavage rules of these impurities. METHODS: Agilent ZORBAX SB-C8 column (150 mm × 3.0 mm, 3.5 μm) was used as the mobile phase. The mobile phase consisted of 5 mmol·L-1 ammonium acetate solution (25:75) 4000 Q TRAP LC / MS / MS for on-line mass spectrometry analysis of clindamycin palmitate hydrochloride. Results: The 10 impurities of clindamycin palmitate hydrochloride were deduced by multi-stage mass spectrometry cleavage as clindamycin, triadimefon, sulfoxide clindamycin palmitate, clindamycin Dodecanoate, ethyl palmitate, clindamycin myristate, clindamycin B palmitate, clindamycin palmitate, clindamycin octadecanoate, Mycophenolate palmitate. Conclusion: The structure of 10 impurities in Clindamycin Hydrochloride Palmitate API was identified, among which 3 impurities were new impurities.