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目的:建立LC-MS方法检测盐酸克林霉素中有关物质,并利用质谱对有关物质进行初步鉴定。方法:液相色谱条件:色谱柱为Diamonsil C18(250 mm×4.6 mm,5μm);流动相为乙腈-四氢呋喃-水-无水甲酸(18∶3∶79∶0.2),氨水调pH为5.45±0.02;流速:1.0 mL.min-1;检测波长:210 nm;柱温为室温;质谱条件:电喷雾电离源正离子检测;源温80℃;锥孔电压35 V。结果:检测出盐酸克林霉素原料中6个有关物质,分别为林可霉素异构体(1)、林可霉素(2)、克林霉素B(3)、7-表克林霉素(4)、克林霉素异构体(5)及去氢克林霉素(6)。除林可霉素、克林霉素B和7-表克林霉素外,其余均未被各国药典收载。结论:本文采用液质联用法,灵敏度高,分离度好,能用于盐酸克林霉素的质量控制及其代谢产物的研究。
OBJECTIVE: To establish a LC-MS method for the determination of clindamycin hydrochloride-related substances and the preliminary identification of related substances by mass spectrometry. Methods: The HPLC conditions were as follows: Diamonsil C18 (250 mm × 4.6 mm, 5 μm) was used as the mobile phase. The mobile phase consisted of acetonitrile-tetrahydrofuran-water- 0.02; flow rate: 1.0 mL.min-1; detection wavelength: 210 nm; column temperature at room temperature; mass spectrometry conditions: electrospray ionization source positive ion detection; source temperature 80 ℃; Results: Six related substances in clindamycin hydrochloride were detected, including lincomycin isomers (1), lincomycin (2), clindamycin B (3), 7- Clindamycin (4), clindamycin isomer (5), and clindamycin (6). In addition to lincomycin, clindamycin B and 7-table clindamycin, the rest are not included in the Pharmacopoeia of each country. Conclusion: In this paper, LC-MS method with high sensitivity and good resolution can be used to study the quality control of clindamycin hydrochloride and its metabolites.