盐酸洛美沙星光降解杂质研究以及盐酸洛美沙星注射剂有关物质的检测  

Studies on photodegradation impurities of lomefl oxacin and determination of its related substances in lomeftoxacin hydrochloride injection

作　　者：李晶晶[1] 李文赟[2] 汪玉馨[1] 陆益红[1] 

机构地区：[1]江苏省食品药品检验所,南京210008 [2]成都大学四川抗菌素工业研究所,成都610052

出　　处：《中国抗生素杂志》2014年第11期833-840,共8页Chinese Journal of Antibiotics

摘　　要：目的采用LC-IT/TOF-MS方法对盐酸洛美沙星光降解杂质进行研究,并采用高效液相色谱法测定盐酸洛美沙星注射剂中有关物质。方法用LC-IT/TOF-MS技术分离并鉴定盐酸洛美沙星光降解杂质,并通过化学合成和制备液相的方法得到杂质A(A为8-氟-9-(3-甲基-1-哌嗪基)-6-氧代-2,6-二氢-1H-吡咯并[3,2,1-ij]喹啉-5-羧酸)、杂质B(8-氟-9-(3-甲基-1-哌嗪基)-6-氧代-2,6-二氢-1H-吡咯并[3,2,1-ij]喹啉-5-羧酸)。用HPLC建立有关物质检测方法,用岛津VP-ODS C18(150mm×4.6mm,5μm)色谱柱,流动相:戊烷磺酸钠溶液-甲醇梯度洗脱,检测波长:287nm;柱温:40℃;流速:1.0m L/min。结果制得的杂质A、杂质B的质谱信息与盐酸洛美沙星相应的光降解杂质一致。有关物质HPLC检查法专属性较好,杂质A、B相对主峰保留时间为0.6、1.4,校正因子分别为1.37和2.37。杂质A的检测限为0.3ng,定量限为1ng。杂质B的检测限为1.1ng,定量限为3.3ng。结论有关物质检测方法适于盐酸洛美沙星的质量控制,盐酸洛美沙星注射剂应注意避光以减少光降解杂质的产生。Objective To study on photodegradation products of lomefloxacin by LC-IT/TOF-MS and establish an HPLC method for the determination of its related substancesin in lomefloxacin hydrochloride injection.Methods LC-IT/TOF-MS was used to analyze and identify photodegradation impurities of lomefloxacin.Impurity A [8-chloro-1-ethyl-6-fluoro-7-（3-methylpiperazin-1-yl）-4-oxo-1,4-dihydroquinoline-3-carboxylic acid] and impurity B [8-fluoro-9-（3-methylpiperazin-1-yl）-6-oxo-2,6-dihydro-1H-pyrrolo（3,2,1-ij） quinoline-5-carboxylic acid] were synthesized.C18 column（SHIMADZU VP-ODS 150mm × 4.6mm,5μm） was used,the mobile phase was sodium pentanesulfonate solution-methanol with gradient elution at detection wavelength of 287nm.Results The mass results of impurity A and B were the same as those of corresponding photodegradation impurities.Lomefloxacin and its related substances could be well separated.The relative retention times of impurity A and impurity B were 0.6 and 1.4,and the correction factors were 1.37 and 2.37 respectively.The limit of quantitation of impurity A was 1.0ng and the limit of detection was 0.3ng.The limit ofquantitation of impurity B was 3.3ng and the limit of detection was 1.1ng.Conclusion The method for related substances is suitable for the quality control of lomefloxacin hydrochloride injection.We should pay attention to avoid light to reduce degradation impurities when lomefloxacin hydrochloride injection is used or reserved.

关 键 词：离子阱飞行时间质谱仪 高效液相色谱法 盐酸洛美沙星注射剂 有关物质 

分 类 号：R978[医药卫生—药品]