LC-MS法研究盐酸克林霉素中的有关物质  

LC-MS studies on related substances in clindamycin hydrochloride

作　　者：孙秋实[1] 李悦[1] 王慧敏[1] 覃俐 

机构地区：[1]上海医药工业研究院,上海200040 [2]浙江天台药业有限公司,台州317200

出　　处：《药物分析杂志》2011年第6期1059-1063,共5页Chinese Journal of Pharmaceutical Analysis

基　　金：国家"重大新药创制"科技重大专项资助项目(编号2009ZX09301-007)

摘　　要：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 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.

关 键 词：氯洁霉素 有关物质 林哥霉素 表克林霉素 异构体 液相色谱-质谱 

分 类 号：R917[医药卫生—药物分析学]