反相高效液相色谱法测定苯酰甲硝唑有关物质  

RP-HPLC determination for related substances of metronidazole benzoate

作　　者：徐永丽[1] 孙晓波[1] 周亮[1] 郭科义 

机构地区：[1]天津中安药业有限公司,天津300384 [2]吉林九鑫制药有限公司,吉林132106

出　　处：《药物分析杂志》2007年第10期1646-1648,共3页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立反相高效液相色谱法测定苯酰甲硝唑有关物质。方法:采用双波长检测,梯度洗脱。色谱柱为迪马公司 Dia-monsil^(TM)C_(18)(250mm×4.6mm,5μm);流动相 A 和 B 分别为1.5g·L^(-1)磷酸二氢钾溶液(用1mol·L^(-1)磷酸溶液调 pH3.2)-乙腈(80:20和58:42);流速1.0mL·min^(-1),检测波长为235,315nm,进样量20μL,柱温为室温,外标法和主成分自身对照法计算。结果:杂质 A、杂质 B、杂质 C、苯酰甲硝唑均能达到很好的分离,并分别在1.12～16.8μg·mL^(-1)(r=1.000),1.12～16.8μg·mL^(-1)(r=0.9999),1.0～15.0μg·mL^(-1)(r=1.000),1.04～15.6μg·mL^(-1)(r=0.9992)浓度范围内具有良好的线性关系。杂质 A、杂质 B、杂质 C 的平均回收率(n=9)分别为99.4%,99.6%,99.5%。结论:本法简便、灵敏、准确,专属性强,适合于苯酰甲硝唑有关物质的测定。Objective： To develop an RP - HPLC method for the assay of related substances in metronidazole benzoate. Methods：Using detection of dual wavelengths and gradient elution. The chromatographic conditions included Column DiamonsilTM C18（250 mm×4. 6 mm,5 μm） and 1.5 g · L^-1 KH2PO4（adjusted to pH 3.2 with 1 mol · L^-1 H3 PO4 ）-acetonitrile （80：20 and 58： 42 ） as the mobile phase A and B, at a flow rate of 1.0 mL · min^-1, detected at 315 and 235 nm, the column temperature was room temperature. Results： Impurity A, impurity B, impurity C and metronidazole benzoate respectively had a good linearity in the range of 1.12 - 16.8 μg · mL^-1 （r = 1. 000）, 1.12-16.8 μg · mL^-1 （r =0.9999）,1.0-15.0 μg · mL^-1 （r = 1.000） and 1.04-15.6 μg · mL^-1 （r = 0. 9992） respectively. The average reeovery（n =9） of impurity A,impurity B and impurity C was 99. 4% ,99. 6%, 99. 5% ,respectively. Conclusion：The established method is high selective, simple and accurate. It is suitable for the determination of related substances in metronidazole benzoate.

关 键 词：苯酰甲硝唑 有关物质 反相HPLC法 双波长检测 梯度洗脱 

分 类 号：R917[医药卫生—药物分析学]