HPLC离子对梯度洗脱法同时测定注射用阿莫西林钠/氟氯西林钠的含量和有关物质  

Assay of amoxicillin sodium and flucloxacillin sodium for injection and their related substances by ion-pairs along with gradient elution HPLC method

作　　者：陈悦[1] 

机构地区：[1]浙江省药品检验所,杭州310004

出　　处：《中国抗生素杂志》2004年第1期15-18,共4页Chinese Journal of Antibiotics

摘　　要：目的建立同时测定阿莫西林钠、氟氯西林钠含量与有关物质的HPLC法,使复方制剂中极性差异较大的两种主药以及它们引入的有关物质同时得以洗脱和测定,提高分析效率和结果的可靠性。方法RP-HPLC离子对梯度洗脱法。色谱柱选用HPZorbaxElicpseXDB-C8柱;流动相A为1.4%十六烷基三甲基溴化铵的0.01mol/L磷酸二氢钾溶液(pH6.5)—乙腈(70∶30);流动相B为1.4%十六烷基三甲基溴化铵的0.01mol/L磷酸二氢钾溶液(pH6.5)—乙腈(30∶70);检测波长为254nm;梯度洗脱。结果阿莫西林钠和氟氯西林钠在上述色谱条件下均有合适的保留,含量测定可在15min内完成,有关物质测定可在30min内完成;制剂中的主要杂质或降解产物均与两个主峰实现了良好分离;当进样体积为10μl时,阿莫西林在0.0088～2.210mg/ml浓度范围内与峰面积有良好的线性关系,氟氯西林在0.0097～2.430mg/ml浓度范围内与峰面积有良好的线性关系;方法的准确性、重复性和专属性令人满意。结论本法可用于注射用阿莫西林钠和氟氯西林钠的含量和有关物质测定。Objective To establish an HPLC method for simultaneous assaying of amoxicillin sodium and flucloxacillin sodium for injection and their related substances.Method Ion-pairs along with gradient elution HPLC method was proposed.The separation was performed on an HP Zorbax Elicpse XDB-C8 column (4.6mm×150mm);The mobile phase A composed of 0.01mol/L KH2PO4 buffer solution (pH 6.5) containing 1.4%cetyl trimethyl ammonium bromide∶acetonitrile (70∶30);mobile phase B composed of 0.01mol/L KH2PO4 buffer solution (pH6.5) containing 1.4%cetyl trimethyl ammonium bromide∶acetonitrile(30∶70).The detection was carried out on a UV detector at 254nm;at a flow rate is about 1ml/min by gradient elution.Results Under the chromatographic system described above amoxicillin and flucloxacillin all have acceptable responses at this wavelength with suitable chromatographic retention on the column.The main impurities of the product for injection were all separated successsively under the gradient elution system;When the injection volume was 10μl,the standard curves of amoxicillin and flucloxacillin were all linear in the range of 0.0088～2.210mg/ml (r=0.99999,n=10) and of 0.0097～2.430 mg/ml(r=0.99997,n=10) respectively.The RSD for repetition was 1.3%and 0.6%,and the average recovery rate of amoxicillin and flucloxacillin was 100.27%and 100.54%respectively (n=9).Conclusion This method offered a rapid,repeatable and accurate procedure convenient for assaying amoxicillin and flucloxacillin simultaneously as well as for determining their impurities.

关 键 词：阿莫西林/氟氯西林 有关物质 离子对 梯度洗脱 高效液相色谱 

分 类 号：R917[医药卫生—药物分析学]