LC-MS法研究盐酸克林霉素中的有关物质

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,5 μm);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 set up an LC-MS method in order to detect the related substances in clindamycin hydrochloride and to identify those related substances by MS. Methods: LC:Diamonsil C₁₈(250 mm×4.6 mm,5 μm)was adopted.The mobile phase consisted of acetonitrile-THF-water-anhydrous formic acid(18∶ 3∶ 79∶ 0.2),and adjust pH to 5.45±0.02 with ammonia.The flow rate was 1.0 mL·min^-1,detection wavelength was 210 nm.The test was carried out under room temperature.MS:positive electrospray ionization (ESI⁺);the source temperature was 80 ℃,and cone voltage was 35 V. Results: Six related substances has been detected in the clindamycin hydrochloride drug substance as isomer of lincomycin(1),lincomycin(2),clindamycin B(3),7-epiclindamycin(4),isomer of clindamycin(5) and dehydroclindamycin(6).The others haven't been collected by pharmacopoeia except for lincomycin,clindamycin B and 7-epiclindamycin. Conclusion: This paper uses LC-MS method,which has the characteristics of high sensitivity and good separation.It proves that this method can be used in the study of quality control and metabolites of clindamycin hydrochloride.