中国抗生素杂志
中國抗生素雜誌
중국항생소잡지
CHINESE JOURNAL OF ANTIBIOTICS
2009年
12期
734-738,742
,共6页
氨苄西林钠舒巴坦钠复方制剂%有关物质%HPLC梯度洗脱法%质量标准
氨芐西林鈉舒巴坦鈉複方製劑%有關物質%HPLC梯度洗脫法%質量標準
안변서림납서파탄납복방제제%유관물질%HPLC제도세탈법%질량표준
Ampicillin sodium/sulbactam sodium%Related substances%HPLC gradient elution%Quality specification
目的 建立有效的注射用氨苄西林钠舒巴坦钠有关物质检测方法.方法 采用HPLC梯度洗脱法,色谱柱为Phenomenex C_(18)(2)型Luna色谱柱,以0.02mol/L磷酸二氢钠溶液pH(4.0±0.1)为流动相A、乙腈为流动相B;流速为1.0ml/min;检测波长为230nm和254nm,采用双波长检测分区域计算.对舒巴坦主峰前的杂质峰,采用230nm的峰面积值按舒巴坦计算其含量;对舒巴坦主峰后的杂质峰,采用254nm的峰面积值按氨苄西林计算其含量.结果 采用梯度洗脱方式能有效检测出氨苄西林二聚物、舒巴坦青霉胺等杂质;不同来源的杂质具有明显分区,与氨苄西林有关的杂质主要集中在舒巴坦主峰后,而与舒巴坦有关的杂质则集中在舒巴坦主峰前;采用双波长分区域检测杂质含量,可以将复方制剂中的有关物质含量同其原料氨苄西林钠和舒巴坦钠中的有关物质含量相联系.各杂质在不同波长下响应值不同.结论 改进后的方法可较好的分离氨苄西林钠和舒巴坦钠来源的各主要杂质,真实反映药品质量,有助于发现目前产品中的质量问题,进而促使产品质量的提高.
目的 建立有效的註射用氨芐西林鈉舒巴坦鈉有關物質檢測方法.方法 採用HPLC梯度洗脫法,色譜柱為Phenomenex C_(18)(2)型Luna色譜柱,以0.02mol/L燐痠二氫鈉溶液pH(4.0±0.1)為流動相A、乙腈為流動相B;流速為1.0ml/min;檢測波長為230nm和254nm,採用雙波長檢測分區域計算.對舒巴坦主峰前的雜質峰,採用230nm的峰麵積值按舒巴坦計算其含量;對舒巴坦主峰後的雜質峰,採用254nm的峰麵積值按氨芐西林計算其含量.結果 採用梯度洗脫方式能有效檢測齣氨芐西林二聚物、舒巴坦青黴胺等雜質;不同來源的雜質具有明顯分區,與氨芐西林有關的雜質主要集中在舒巴坦主峰後,而與舒巴坦有關的雜質則集中在舒巴坦主峰前;採用雙波長分區域檢測雜質含量,可以將複方製劑中的有關物質含量同其原料氨芐西林鈉和舒巴坦鈉中的有關物質含量相聯繫.各雜質在不同波長下響應值不同.結論 改進後的方法可較好的分離氨芐西林鈉和舒巴坦鈉來源的各主要雜質,真實反映藥品質量,有助于髮現目前產品中的質量問題,進而促使產品質量的提高.
목적 건립유효적주사용안변서림납서파탄납유관물질검측방법.방법 채용HPLC제도세탈법,색보주위Phenomenex C_(18)(2)형Luna색보주,이0.02mol/L린산이경납용액pH(4.0±0.1)위류동상A、을정위류동상B;류속위1.0ml/min;검측파장위230nm화254nm,채용쌍파장검측분구역계산.대서파탄주봉전적잡질봉,채용230nm적봉면적치안서파탄계산기함량;대서파탄주봉후적잡질봉,채용254nm적봉면적치안안변서림계산기함량.결과 채용제도세탈방식능유효검측출안변서림이취물、서파탄청매알등잡질;불동래원적잡질구유명현분구,여안변서림유관적잡질주요집중재서파탄주봉후,이여서파탄유관적잡질칙집중재서파탄주봉전;채용쌍파장분구역검측잡질함량,가이장복방제제중적유관물질함량동기원료안변서림납화서파탄납중적유관물질함량상련계.각잡질재불동파장하향응치불동.결론 개진후적방법가교호적분리안변서림납화서파탄납래원적각주요잡질,진실반영약품질량,유조우발현목전산품중적질량문제,진이촉사산품질량적제고.
Objective To development the method of separating and determining the related substances for injection of ampicillin sodium/sulbactam sodium.Methods HPLC gradient elution was performed by using Phenomenex C_(18)(2)colum,named Luna.The mobile phase was consisted of A,0.02 mol/L phosphate buffer(pH4.0 ±0.1);and B,acetonitrile.The flow rate was 1.0ml/min,the detection wavelength was 230nm/254nm.The concentration of related substances Was quantified in different division by double wavelengths.The impurities of sulbactam,before the main peak of sulbactam,was quantified by external standard method of reference sulbactam in 230nm,and the impurities of ampicillin,after the main peak of sulbactam,Was quantified by external standard method of reference ampicillin at 254nm.Results The isocratic elution method was available for detecting ampicillin dimer,(2S)2-amino-3-methyl-3-sulphinobutanoic acid and other impurities.The impurities from different sources had obvious division,and the impurities of ampicillin mainly the peak of sulbactam,the impurities of sulbactam mainly before this peak.It Was able to relate the result of related substances in the injection with the impurities in the sinsle drug of ampicilln or suhactam,that detected in different division by double wavelengths.Conclusion The improved method can be used to separate the related substances from different components,and is suitable for controlling the quality of this drug.
